CN106435497B - A kind of energy saving fenestrated membrane of golden low radiation and preparation method thereof - Google Patents

A kind of energy saving fenestrated membrane of golden low radiation and preparation method thereof Download PDF

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CN106435497B
CN106435497B CN201610811946.5A CN201610811946A CN106435497B CN 106435497 B CN106435497 B CN 106435497B CN 201610811946 A CN201610811946 A CN 201610811946A CN 106435497 B CN106435497 B CN 106435497B
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layer
thickness
refractive index
fenestrated membrane
high refractive
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CN106435497A (en
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吴培服
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Jiangsu Shuangxing Color Plastic New Materials Co Ltd
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Jiangsu Shuangxing Color Plastic New Materials Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C23C14/0652—Silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering

Abstract

The present invention proposes a kind of energy saving fenestrated membrane of golden low radiation and preparation method thereof, and fenestrated membrane is in gold in the sun, and the film layer structure of the gold fenestrated membrane is followed successively by from inside to outside：Flexible and transparent PET base material layer；First high refractive index layer；First metal oxide layer；First ag alloy layer；First barrier layer；Second high refractive index layer；Second metal oxide layer；Second ag alloy layer；Second barrier layer；Third high refractive index layer.Reflection of the fenestrated membrane of the present invention by the double-deck ag alloy layer to infrared light forms index matching relationship with three floor height refracting layers, and by the cooperation of thickness parameter, color is viewed as gold under sunlight, has excellent visual effect.Meanwhile the gold fenestrated membrane also has excellent light transmission, heat-insulated and antioxygenic property, service life is long, is readily produced.

Description

A kind of energy saving fenestrated membrane of golden low radiation and preparation method thereof
Technical field
The present invention relates to the pad pasting being attached on the glass pane of automobile, building etc., in gold under especially a kind of sunlight Fenestrated membrane, more particularly to a kind of energy saving fenestrated membrane of golden low radiation and preparation method thereof.
Background technology
It is frequently necessary to attach pad pasting, commonly referred to as fenestrated membrane on the glass pane of automobile, building etc., to provide heat-insulated, anti-purple The functions such as outside line.Meanwhile the fenestrated membrane haveing excellent performance can also provide good visible light transmittance rate, it can be from the inside of glass pane Outside clear observation window.Wherein, Low emissivity fenestrated membrane is also known as Low-E fenestrated membranes, is to deposit Low emissivity film layer in flexible and transparent substrate surface It forms；Low emissivity fenestrated membrane has higher light transmittance to visible light, meanwhile, there is very high reflectivity to infrared ray and ultraviolet light, Be it is a kind of have both high light transmission, it is high heat-insulated the advantages that film product.
Currently, the energy saving fenestrated membrane of traditional Low emissivity there is colors single, some disadvantages such as heat-proof quality difference, and have The energy saving fenestrated membrane of golden low radiation of very strong decorative effect is even more rare.Current most fenestrated membrane is all that the poor heat of energy saving is anti- Coating fenestrated membrane is penetrated, structural stability is poor, and heat insulation is bad, and service life is shorter, is unfavorable for product and promotes on a large scale.
In the industrial production of the energy saving fenestrated membrane of Low emissivity, the magnetic control fenestrated membrane production later stage, which also needs to be coated technique, is answered Close, this makes fenestrated membrane inevitably be contacted with air, to cause its oxidation, and in transportational process temperature variation, Also the oxidation that will accelerate fenestrated membrane, directly affects its service life.
Invention content
The technical problem to be solved in the present invention is to provide energy saving fenestrated membranes of a kind of golden low radiation and preparation method thereof, to reduce Or it avoids the problem that being formerly mentioned.
In order to solve the above technical problems, the present invention proposes a kind of energy saving fenestrated membrane of golden low radiation, it is in gold in the sun, The film layer structure of the fenestrated membrane is followed successively by from inside to outside：Flexible and transparent PET base material layer, thickness are 23 microns~50 microns, can Light-exposed light transmittance >=89%, mist degree≤1.5；First high refractive index layer, thickness are 28nm~30nm, and refractive index 2.06 is described First high refractive index layer is by Si3N4It constitutes；First metal oxide layer, thickness are 3nm~6nm, first metal oxide layer By ZnO:Al is constituted；First ag alloy layer, thickness are 11nm~13nm, and first ag alloy layer is by 98% Ag, 2% Pd It constitutes；First barrier layer, thickness are 0.8nm~1.5nm, and first barrier layer is made of Si；Second high refractive index layer, thickness For 56nm~60nm, refractive index 2.36, second high refractive index layer is by Nb2O5It constitutes；Second metal oxide layer, thickness For 6nm~8nm, second metal oxide layer is by ZnO:Al is constituted；Second ag alloy layer, thickness be 14.5nm~ 16.5nm, second ag alloy layer is by 98% Ag, 2% Pd compositions；Second barrier layer, thickness is 1nm~2nm, described Second barrier layer is made of Si；Third high refractive index layer, thickness are 25nm~27nm, refractive index 2.06, the third height folding Rate layer is penetrated by Si3N4It constitutes.
Preferably, the thickness of first metal oxide layer is less than or equal to the 2/3 of the thickness of first ag alloy layer； The thickness of second metal oxide layer is less than or equal to the 2/3 of the thickness of second ag alloy layer.
Preferably, the thickness of first barrier layer is less than or equal to the 1/5 of the thickness of first ag alloy layer；Described The thickness of two barrier layers is less than or equal to the 1/5 of the thickness of second ag alloy layer.
Preferably, the thickness of the flexible and transparent PET base material layer is 23 microns；The thickness of first high refractive index layer is 29nm；The thickness of first metal oxide layer is 5nm；The thickness of first ag alloy layer is 12nm；First resistance The thickness of interlayer is 1.2nm；The thickness of second high refractive index layer is 58nm；The thickness of second metal oxide layer is 7nm；The second ag alloy layer thickness is 15nm；The thickness of second barrier layer is 1.5nm；The third high refractive index layer Thickness be 26nm.
Preferably, the energy saving fenestrated membrane of the golden low radiation is 72.2%, is in wavelength in the light transmittance of visible-range The light transmittance of the infrared region of 780nm~2500nm is 8.9%, is that infrared barrier rate at 950nm wavelength is in wavelength 85.3%, be infrared barrier rate at 1400nm wavelength in wavelength it is 95.2%.
The present invention also provides a kind of preparation methods of the above-mentioned energy saving fenestrated membrane of golden low radiation, include the following steps：
(1) flexible and transparent PET film is provided as the flexible and transparent PET base material layer；
(2) it is deposited in the flexible and transparent PET base material layer by way of dual rotary cathode, MF reactive magnetron sputtering First high refractive index layer；
(3) by way of single rotating cathode, direct current reaction magnetron sputtering institute is deposited on first high refractive index layer State the first metal oxide layer；
(4) it is deposited on first metal oxide layer by way of monoplane cathode, direct current reaction magnetron sputtering First ag alloy layer；
(5) described in being deposited on first ag alloy layer by way of monoplane cathode, direct current reaction magnetron sputtering First barrier layer；
(6) described is deposited on first barrier layer by way of dual rotary cathode, MF reactive magnetron sputtering Two high refractive index layers；
(7) by way of single rotating cathode, direct current reaction magnetron sputtering institute is deposited on second high refractive index layer State the second metal oxide layer；
(8) it is deposited on second metal oxide layer by way of monoplane cathode, direct current reaction magnetron sputtering Second ag alloy layer；
(9) described in being deposited on second ag alloy layer by way of monoplane cathode, direct current reaction magnetron sputtering Second barrier layer；
(10) described is deposited on second barrier layer by way of dual rotary cathode, MF reactive magnetron sputtering Three high refractive index layers.
Preferably, in magnetron sputtering deposition plated film, all indoor temperature of chamber are constant at -15 DEG C~15 DEG C respectively.
Preferably, the step (2), step (3), step (6), step (7), step (10) include：In corresponding chambers It is 10 to be passed through volume ratio:1~100:1 argon gas and the mixed gas of oxygen, setting sputtering vacuum degree 10-6Torr, plated film are stablized Air pressure is 10-3Torr；Dual rotary cathode, MF reactive magnetron sputtering power are 20Kw~50Kw；Single rotating cathode, direct current reaction Magnetron sputtering power is 2Kw~5Kw.
Preferably, the step (4), step (5), step (8), step (9) include：Purity is passed through in corresponding chambers not Argon gas less than 99.99%, setting sputtering vacuum degree 10-6Torr, it is 10 that plated film, which stablizes air pressure,-3Torr；It is monoplane cathode, straight Stream reaction magnetocontrol sputtering power is 0.5Kw~8Kw.
Preferably, the step 4 further comprises, by way of the UV masks that horizontal parallel arranges are arranged, in institute State first ag alloy layer for the striated that horizontal direction parallel arrangement is formed on the first metal oxide layer.The step 8 Further comprise, in such a way that the UV masks that horizontal parallel arranges are set, is formed on second metal oxide layer Second ag alloy layer of the striated of horizontal direction parallel arrangement.The horizontal direction parallel of second ag alloy layer arranges Striped and first ag alloy layer horizontal direction parallel arrangement striped be preferably staggeredly arranged.
Beneficial effects of the present invention
Compared with prior art, there is the energy saving fenestrated membrane of the golden low radiation of 9 layers of coating structure the present invention provides a kind of Structurally consummate, performance is stablized, and can effectively overcome the disadvantage of the prior art, the function of ag alloy layer is made effectively to be sent out It waves, higher visible light transmittance rate is kept while infrared emittance is greatly reduced.Golden low radiation provided by the invention is energy saving Fenestrated membrane preparation method is simple for process, easy to operate, it is easy to accomplish mass production.
The energy saving fenestrated membrane of golden low radiation provided by the invention, traditional silver layer is replaced using ag alloy layer, is had preferable Inoxidizability.
The energy saving fenestrated membrane of golden low radiation provided by the invention, makees place mat using oxide skin(coating) for ag alloy layer；Oxide Layer can promote the growth of silver alloy film that it is made to grow up to continuous structure as early as possible, and very thin metal layer can have very high red in this way External reflectance rate and preferable visible light transmittance.
The energy saving fenestrated membrane of golden low radiation provided by the invention, protects ag alloy layer using barrier layer, it is ensured that The reflectivity of infrared light will not be reduced with the extension of usage time, extend the service life of fenestrated membrane, have lasting height Heat insulation.
The energy saving fenestrated membrane of golden low radiation provided by the invention, passes through the rational design of 9 tunic layer thickness, coating material itself The interference between film layer of characteristic and light, barrier ultraviolet light and infrared ray while realizing the high transmission of visible light, and Improve its colour cast effect, realizes golden film surface color.
In short, reflection of the fenestrated membrane of the present invention by the double-deck ag alloy layer to infrared light, forms with three floor height refracting layers and rolls over Rate matching relationship is penetrated, and by the cooperation of thickness parameter, color is viewed as gold under sunlight, has excellent vision Effect.Meanwhile the gold fenestrated membrane also has excellent light transmission, heat-insulated and antioxygenic property, service life is long, is readily produced.
Description of the drawings
The following drawings are only intended to schematically illustrate and explain the present invention, not delimit the scope of the invention.Wherein,
The layer structural representation of the energy saving fenestrated membrane of golden low radiation of a specific embodiment according to the present invention is shown in Fig. 1 Figure；
The light transmittance curve figure of the energy saving fenestrated membrane of golden low radiation shown in Fig. 1 is shown in Fig. 2；
The reflectance curve figure of the energy saving fenestrated membrane of golden low radiation shown in Fig. 1 is shown in Fig. 3.
Specific implementation mode
For a clearer understanding of the technical characteristics, objects and effects of the present invention, now control illustrates this hair Bright specific implementation mode.Wherein, identical component uses identical label.
The schematic diagram of a layer structure of the golden fenestrated membrane of the present invention as shown in Figure 1, film layer structure are followed successively by from inside to outside：It is flexible Transparent PET substrate layer 1, thickness are 23 microns~50 microns, visible light transmittance rate >=89%, mist degree≤1.5, and preferred thickness is 23 microns；First high refractive index layer 2, thickness be 28nm~30nm, refractive index 2.06, first high refractive index layer 2 by Si3N4It constitutes, preferred thickness 29nm；First metal oxide layer 3, thickness are 3nm~6nm, first metal oxide layer 3 by ZnO:Al is constituted, preferred thickness 5nm；First ag alloy layer 4, thickness are 11nm~13nm, first ag alloy layer 4 By 98% Ag, 2% Pd is constituted, preferred thickness 12nm；First barrier layer 5, thickness be 0.8nm~1.5nm, described first Barrier layer 5 is made of Si, preferred thickness 1.2nm；Second high refractive index layer 6, thickness are 56nm~60nm, and refractive index is 2.36, second high refractive index layer 6 is by Nb2O5It constitutes, preferred thickness 58nm；Second metal oxide layer 7, thickness 6nm ~8nm, second metal oxide layer 7 is by ZnO:Al is constituted, preferred thickness 7nm；Second ag alloy layer 8, thickness are 14.5nm~16.5nm, second ag alloy layer 8 is by 98% Ag, 2% Pd compositions, preferred thickness 15nm；Second resistance Interlayer 9, thickness are 1nm~2nm, and second barrier layer 9 is made of Si, preferred thickness 1.5nm；Third high refractive index layer 10, thickness is 25nm~27nm, and refractive index 2.06, the third high refractive index layer 10 is by Si3N4It constitutes, preferred thickness is 26nm。
The following detailed description of the preparation process of the golden fenestrated membrane of the present invention：
(1) flexible and transparent PET film is provided first as the flexible and transparent PET base material layer 1.In a specific embodiment In, in order to obtain more preferably light transmittance, visible light transmittance rate >=89% of the flexible and transparent PET base material layer 1, mist can be selected Degree≤1.5.
(2) deposition first is high in the PET base material layer 1 by way of dual rotary cathode, MF reactive magnetron sputtering rolls over Penetrate rate layer 2, the refractive index of preferably first high refractive index layer 2 is 2.06.The present invention is by way of magnetron sputtering in PET film Upper Direct precipitation is by Si3N4The first high refractive index layer 2 constituted, due to Si3N4There is good adhesive force between PET film, adopt Use Si3N4It can be handled without carrying out additional metal coating to PET film to improve adhesive force with Direct precipitation on a pet film, from And the number of plies can be reduced and improve translucency, while if handled using metal coating, the color of the fenestrated membrane of the present invention can be destroyed, Desired gold can not be obtained.
(3) by way of single rotating cathode, direct current reaction magnetron sputtering first is deposited on first high refractive index layer 2 Metal oxide layer 3.Two layers of ZnO is used in the golden fenestrated membrane of the present invention:Al layers (zinc oxide films of aluminium doping), referring to step 7.ZnO:Al layers of thickness very little, only several nanometers, but the ZnO of these nano thickness:Al layers can promote follow-up silver The growth of alloy-layer makes it grow up to continuous compact texture as early as possible, thus significantly reduces the thickness of follow-up ag alloy layer, improves window The translucency of film.Fine and close ag alloy layer can effectively reflect infrared ray and ultraviolet light simultaneously, improve the heat-proof quality of fenestrated membrane. In one preferred embodiment, every layer of ZnO:Al layers of thickness is less than or equal to the 2/3 of the thickness of follow-up ag alloy layer, you can obtains excellent The translucency and heat-proof quality of choosing.Also that is, the thickness of the first metal oxide layer 3 is less than or equal to the thickness of the first ag alloy layer 4 The 2/3 of degree；The thickness of second metal oxide layer 7 is less than or equal to the 2/3 of the thickness of the second ag alloy layer 8.
(4) is deposited on first metal oxide layer 3 by way of monoplane cathode, direct current reaction magnetron sputtering One ag alloy layer 4.It is preferred that the ag alloy layer includes 98% Ag, the Pd that surplus is 2% can be obtained more preferable with respect to fine silver Antioxygenic property and moisture protection, certainly, the setting of ag alloy layer is mainly used for carrying out infrared ray and ultraviolet light anti- It penetrates to provide excellent heat-proof quality.Simultaneously it should be pointed out that since the thickness of ag alloy layer is more than or equal to ZnO below:Al The 3/2 of the thickness of layer, and the consistency of the ag alloy layer formed is higher, thus the color of the fenestrated membrane of the present invention is by silver alloy The thickness of layer is affected, certainly, for the setting of the double-deck ag alloy layer of the present invention, between two layers of ag alloy layer The index matching relationship of spacing and three floor height refracting layers, and the indispensable factor of the color of golden fenestrated membrane is obtained, This is described in detail below.
In a preferred embodiment, in step 4, can be arranged horizontal parallel arrange UV masks by way of, The first ag alloy layer 4 is deposited on the first metal oxide layer 3, then removes UV masks, forms horizontal direction parallel arrangement Striated the first ag alloy layer 4.Such as the generation type of UV masks can be, one is sprayed in the first metal oxide layer 3 Layer UV glue, then irradiates UV glue behind horizontally arranged stripe grating using UV light, keeps the UV glue for the part being illuminated solid Change, uncured UV glue is removed, forms the UV masks of horizontal parallel arrangement.
Horizontal direction parallel arrangement striated the first ag alloy layer 4 can be formed in the longitudinal direction different light transmittances and Reflectivity, but the sight of parallel direction is had no effect on, thus when user is from glass pane inside is close to glass pane outward When, user's sight is nearly horizontal perpendicular to stripe direction, thus can't influence outside sight.And on the outside of glass pane Personnel when observe, usually distance farther out, thus is easy the shadow by longitudinal different light transmittances and reflectivity It rings, causes blurred vision, image mottled, so as to prevent from peeping.
(5) the first resistance of deposition on first ag alloy layer 4 by way of monoplane cathode, direct current reaction magnetron sputtering Interlayer 5.First barrier layer 5 for being protected to the first ag alloy layer 4, avoid the first ag alloy layer 4 aoxidize and light transmission and Reflecting properties reduce, it is ensured that the reflectivity of the infrared light of ag alloy layer will not be reduced with the extension of usage time, be extended The service life of fenestrated membrane has lasting high heat insulation.In a preferred embodiment, the thickness of the first barrier layer 5 is less than Equal to the 1/5 of the thickness of the first ag alloy layer 4 below, which can utilize the first barrier layer 5 of minimum thickness The antioxygenic property needed is obtained, thus optimal heat insulation can be obtained with minimum thickness, improves the entirety of fenestrated membrane Light transmission.
(6) deposition second is high on first barrier layer 5 by way of dual rotary cathode, MF reactive magnetron sputtering rolls over Penetrate rate layer 6, the refractive index of preferably second high refractive index layer 6 is 2.36.The thickness of second high refractive index layer 6 of this step and The relatively other high refractive index layers of refractive index will be big, i.e., for the double-deck ag alloy layer of the present invention, two layers of silver alloy Second high refractive index layer 6 of bigger refractive index is set between layer, the interval shape between smaller two layers of ag alloy layer can be utilized At the bireflectance structure of reflection infrared ray and ultraviolet light, thus the thickness of the second high refractive index layer 6 can be reduced, improve fenestrated membrane Integral light-transmitting performance.
(7) by way of single rotating cathode, direct current reaction magnetron sputtering second is deposited on second high refractive index layer 6 Metal oxide layer 7.The thickness of the second metal oxide layer 7 deposited in this step is than the first metal oxygen in abovementioned steps 3 The thickness of compound layer 3 is bigger, to reflect more infrared rays and ultraviolet light by the second ag alloy layer 8 of thicker outer layer, The second ag alloy layer 8 that outer layer can be penetrated is reduced, thus the first ag alloy layer 4 of internal layer can be arranged thinner by one A bit, the thickness of corresponding first metal oxide layer 3 can also become smaller.Pass through the first metal oxide layer 3 and the second metal oxygen The thickness matching of compound layer 7, can improve the optical homogeneity of fenestrated membrane, but most significant effect be can be to the window of the present invention The coloration of film is adjusted, that is, the gold of golden fenestrated membrane of the invention, mainly by the first metal oxide layer 3 and the second metal The thickness proportion relationship of oxide skin(coating) 7 and the first ag alloy layer 4 and the second ag alloy layer 8 thereon is determined.This is this hair The bright best parameter group for being different from other technologies, the prior art there is no any scheme to provide the parameter combination for obtaining golden fenestrated membrane Principle, the parameter combination right and wrong are it will be apparent that have substantive distinguishing features outstanding and significant progress.
(8) is deposited on second metal oxide layer 7 by way of monoplane cathode, direct current reaction magnetron sputtering Two ag alloy layers 8.It is preferred that the ag alloy layer includes 98% Ag, the Pd that surplus is 2%.The setting of second ag alloy layer 8 The bireflectance structure for foring reflection infrared ray and ultraviolet light, reduces fenestrated membrane thickness, improves light transmission, strengthen simultaneously Heat-proof quality.
Similar, as in step 4, in a preferred embodiment, in the magnetron sputtering process of step 8, In such a way that the UV masks that horizontal parallel arranges are set the second ag alloy layer can be deposited on the second metal oxide layer 7 8, then UV masks are removed, form the second ag alloy layer 8 of the striated of horizontal direction parallel arrangement.Form the side of UV masks Formula is as previously mentioned, be not repeated.
However, the striped and the first ag alloy layer 4 of the horizontal direction parallel arrangement for the second ag alloy layer 8 that this step is formed Horizontal direction parallel arrangement striped be preferably staggeredly arranged, that is, the first silver alloy of striped face of the second ag alloy layer 8 The gap of the striped of layer 4, the striped of the first ag alloy layer of gap face 4 of the striped of the second ag alloy layer 8.It is preferred at another It in embodiment, can be arranged that width of fringe is identical as interval width, be convenient for the setting of striped mask in this way, while also allow for two layers Striped is just staggeredly arranged, and it is easy to process can to simplify technique.
Respective gap is covered up by the striped being staggeredly arranged, it can be to avoid heat-insulated and reflecting effect due to gap Presence and reduce.Meanwhile the striped being staggeredly arranged so that close to glass pane observation when (within 1 meter), light transmittance and Reflectivity is almost identical, that is, is barely detectable the presence of striped from outside to inside and from inside to outside, and from 1 meter with When outer observation, since the presence of sight angle can generate anti-peeping effect.Meanwhile the ag alloy layer of striated reduces Range of defilade, improves light transmittance, the influence of function and color homogeneity simultaneously for fenestrated membrane is comparatively small.
(9) by way of monoplane cathode, direct current reaction magnetron sputtering on second ag alloy layer 8 deposition the two the One barrier layer 9 is protected to be formed to the second ag alloy layer 8, prevents from aoxidizing, it is ensured that the reflectivity of the infrared light of ag alloy layer is not It can be reduced with the extension of usage time, extend the service life of fenestrated membrane, there is lasting high heat insulation.It is excellent at one The thickness of the two the first barrier layers 9 is selected in embodiment to be less than or equal to the 1/5 of the thickness of the second ag alloy layer 8 below, the thickness Degree ratio can utilize the two the first barrier layers 9 of minimum thickness to obtain the antioxygenic property needed, thus can use minimum Thickness obtains optimal heat insulation, improves the integral light-transmitting performance of fenestrated membrane.
(10) by way of dual rotary cathode, MF reactive magnetron sputtering is deposited on the two the first barrier layers 9 Three high refractive index layers 10, the preferably refractive index of the third high refractive index layer 10 are 2.06.Outermost third high refractive index layer The infrared light in sunlight is effectively reflected in 10 selections, further improves the heat-proof quality of fenestrated membrane.Meanwhile three floor height refraction The refraction of rate layer and being superimposed for two layers ag alloy layer reflection light ultimately form required golden fenestrated membrane of the invention.
Wherein, when magnetron sputtering deposition plated film, all indoor temperature of chamber are constant, and steady temperature model in all chambers Enclose is -15 DEG C~15 DEG C.
Preferably, the step (2), step (3), step (6), step (7), step (10) include：In corresponding chambers It is 10 to be passed through volume ratio:1~100:1 argon gas and the mixed gas of oxygen, setting sputtering vacuum degree 10-6Torr, plated film are stablized Air pressure is 10-3Torr；Dual rotary cathode, MF reactive magnetron sputtering power are 20Kw~50Kw；Single rotating cathode, direct current reaction Magnetron sputtering power is 2Kw~5Kw.
Preferably, the step (4), step (5), step (8), step (9) include：Purity is passed through in corresponding chambers not Argon gas less than 99.99%, setting sputtering vacuum degree 10-6Torr, it is 10 that plated film, which stablizes air pressure,-3Torr；It is monoplane cathode, straight Stream reaction magnetocontrol sputtering power is 0.5Kw~8Kw.
Golden fenestrated membrane provided by the invention is placed in solar film tester and is tested, as a result as Figure 2-3, is shown respectively What is shown is the light transmittance curve figure and reflectance curve figure of golden fenestrated membrane shown in Fig. 1, shows golden window provided by the invention in figure Film is 72.2% in the light transmittance of visible-range；The light transmittance of infrared region for being 780nm~2500nm in wavelength is 8.9%.In addition, by test, gold fenestrated membrane provided by the invention is that infrared barrier rate at 950nm wavelength is in wavelength 85.3%；In wavelength be infrared barrier rate at 1400nm wavelength it is 95.2%, shows that golden fenestrated membrane provided by the invention has Good optical property and heat-proof quality.
This golden fenestrated membrane provided by the invention is placed in spectrophotometer and tests its color.Through color, reflected colour Color is characterized by CIELAB color space index systems, and wherein L* represents brightness, bright, the small expression of numerical value of the big expression of numerical value Secretly；A* represents red green degree, and wherein a* is negative to be represented green, and numerical value is bigger to indicate greener, and a* is just representing red, and numerical value is bigger to indicate redder； B* represents champac degree, and wherein b* is negative to represent indigo plant, and numerical value is bigger to indicate more blue, and b* just represents Huang, and numerical value is bigger to indicate more yellow.Through Color be out of automobile, in building through the color that can be seen when external scene in terms of the glass after pad pasting；Reflected colour is from automobile Outside, outside building the color that can be seen when internal scenery is seen through the glass after pad pasting.By test, gold provided by the invention Fenestrated membrane passes through multiple spot retest in spectrophotometer, penetrates the a*=-1.88, b*=2.17, the a*=- of reflected colour of color 1.03, b*=-2.56, color is viewed as gold under sunlight, and reflected spectral range is 550nm~760nm, is had exhausted Good visual effect.
In conclusion reflection of the fenestrated membrane of the present invention by the double-deck ag alloy layer to infrared light, with three floor height refracting layer shapes At index matching relationship, and by the cooperation of thickness parameter, color is viewed as gold under sunlight, has excellent Visual effect.Meanwhile the gold fenestrated membrane also has excellent light transmission, heat-insulated and antioxygenic property, service life is long, is easy to raw It produces and promotes the use of.
It will be appreciated by those skilled in the art that although the present invention is described in the way of multiple embodiments, It is that not each embodiment only contains an independent technical solution.So narration is used for the purpose of for the sake of understanding in specification, The skilled in the art should refer to the specification as a whole is understood, and by technical solution involved in each embodiment Regard as and can be combined with each other into the mode of different embodiments to understand protection scope of the present invention.
The foregoing is merely the schematical specific implementation modes of the present invention, are not limited to the scope of the present invention.It is any Those skilled in the art, do not depart from the design of the present invention and under the premise of principle made by equivalent variations, modification and combination, The scope of protection of the invention should all be belonged to.

Claims (9)

1. a kind of energy saving fenestrated membrane of golden low radiation is in gold in the sun, which is characterized in that the film layer structure of the fenestrated membrane is by interior It is followed successively by outward：
Flexible and transparent PET base material layer (1), thickness are 23 microns~50 microns, visible light transmittance rate >=89%, mist degree≤1.5；
First high refractive index layer (2), thickness be 28nm~30nm, refractive index 2.06, first high refractive index layer (2) by Si3N4It constitutes；
First metal oxide layer (3), thickness are 3nm~6nm, and first metal oxide layer (3) is by ZnO:Al is constituted；
The first ag alloy layer (4) of the striated of horizontal direction parallel arrangement, thickness are 11nm~13nm, first silver alloy Layer (4) is by 98% Ag, 2% Pd compositions；
First barrier layer (5), thickness are 0.8nm~1.5nm, and first barrier layer (5) is made of Si；
Second high refractive index layer (6), thickness be 56nm~60nm, refractive index 2.36, second high refractive index layer (6) by Nb2O5It constitutes；
Second metal oxide layer (7), thickness are 6nm~8nm, and second metal oxide layer (7) is by ZnO:Al is constituted；
The second ag alloy layer (8) of the striated of horizontal direction parallel arrangement, thickness are 14.5nm~16.5nm, second silver medal Alloy-layer (8) is by 98% Ag, 2% Pd compositions；Second ag alloy layer (8) horizontal direction parallel arrangement striped with The striped of the horizontal direction parallel arrangement of first ag alloy layer (4) is staggeredly arranged；
Second barrier layer (9), thickness are 1nm~2nm, and second barrier layer (9) is made of Si；
Third high refractive index layer (10), thickness be 25nm~27nm, refractive index 2.06, the third high refractive index layer (10) by Si3N4It constitutes.
2. the energy saving fenestrated membrane of golden low radiation according to claim 1, which is characterized in that first metal oxide layer (3) thickness is less than or equal to the 2/3 of the thickness of first ag alloy layer (4)；The thickness of second metal oxide layer (7) Less than or equal to the 2/3 of the thickness of second ag alloy layer (8).
3. the energy saving fenestrated membrane of golden low radiation according to claim 1, which is characterized in that the thickness of first barrier layer (5) Degree is less than or equal to the 1/5 of the thickness of first ag alloy layer (4)；The thickness of second barrier layer (9) is less than or equal to described The 1/5 of the thickness of second ag alloy layer (8).
4. the energy saving fenestrated membrane of golden low radiation according to claim 1, which is characterized in that the flexible and transparent PET base material layer (1) thickness is 23 microns；The thickness of first high refractive index layer (2) is 29nm；First metal oxide layer (3) Thickness is 5nm；The thickness of first ag alloy layer (4) is 12nm；The thickness of first barrier layer (5) is 1.2nm；It is described The thickness of second high refractive index layer (6) is 58nm；The thickness of second metal oxide layer (7) is 7nm；Second silver medal closes Layer gold (8) thickness is 15nm；The thickness of second barrier layer (9) is 1.5nm；The thickness of the third high refractive index layer (10) For 26nm.
5. the energy saving fenestrated membrane of golden low radiation according to claim 4, which is characterized in that the energy saving fenestrated membrane of golden low radiation The light transmittance of visible-range is 72.2%, the light transmittance of infrared region that is 780nm~2500nm in wavelength is 8.9%, it is that infrared barrier rate at 950nm wavelength is 85.3%, is the infrared barrier at 1400nm wavelength in wavelength in wavelength Rate is 95.2%.
6. a kind of preparation method of the energy saving fenestrated membrane of golden low radiation according to any one of claims 1 to 5, feature exist In including the following steps：
(1) flexible and transparent PET film is provided as the flexible and transparent PET base material layer (1)；
(2) it is deposited on the flexible and transparent PET base material layer (1) by way of dual rotary cathode, MF reactive magnetron sputtering First high refractive index layer (2)；
(3) described in being deposited on first high refractive index layer (2) by way of single rotating cathode, direct current reaction magnetron sputtering First metal oxide layer (3)；
(4) by way of monoplane cathode, direct current reaction magnetron sputtering, the UV masks that setting horizontal parallel arranges, described First ag alloy layer (4) is deposited on first metal oxide layer (3), then removes UV masks, and it is flat to form horizontal direction First ag alloy layer (4) of the striated of row arrangement；
(5) described is deposited on first ag alloy layer (4) by way of monoplane cathode, direct current reaction magnetron sputtering One barrier layer (5)；
(6) by way of dual rotary cathode, MF reactive magnetron sputtering described second is deposited on first barrier layer (5) High refractive index layer (6)；
(7) described in being deposited on second high refractive index layer (6) by way of single rotating cathode, direct current reaction magnetron sputtering Second metal oxide layer (7)；
(8) by way of monoplane cathode, direct current reaction magnetron sputtering, the UV masks that setting horizontal parallel arranges, described Second ag alloy layer (8) is deposited on second metal oxide layer (7), then removes UV masks, and it is flat to form horizontal direction Second ag alloy layer (8) of the striated of row arrangement；
(9) described is deposited on second ag alloy layer (8) by way of monoplane cathode, direct current reaction magnetron sputtering Two barrier layers (9)；
(10) described is deposited on second barrier layer (9) by way of dual rotary cathode, MF reactive magnetron sputtering Three high refractive index layers (10).
7. the preparation method of the energy saving fenestrated membrane of golden low radiation according to claim 6, which is characterized in that heavy in magnetron sputtering When product plated film, all indoor temperature of chamber are constant at -15 DEG C~15 DEG C respectively.
8. the preparation method of the energy saving fenestrated membrane of golden low radiation according to claim 6, which is characterized in that the step (2), Step (3), step (6), step (7), step (10) include：It is 10 that volume ratio is passed through in corresponding chambers:1~100:1 argon The mixed gas of gas and oxygen, setting sputtering vacuum degree 10-6Torr, it is 10 that plated film, which stablizes air pressure,-3Torr；Dual rotary cathode, in Frequency reaction magnetocontrol sputtering power is 20Kw~50Kw；Single rotating cathode, direct current reaction magnetron sputtering power are 2Kw~5Kw.
9. the preparation method of the energy saving fenestrated membrane of golden low radiation according to claim 6, which is characterized in that the step (4), Step (5), step (8), step (9) include：The argon gas that purity is not less than 99.99%, setting sputtering are passed through in corresponding chambers Vacuum degree 10-6Torr, it is 10 that plated film, which stablizes air pressure,-3Torr；Monoplane cathode, direct current reaction magnetron sputtering power be 0.5Kw~ 8Kw。
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