CN104669712A - Ag alloy heat-insulating film and preparation method thereof - Google Patents

Ag alloy heat-insulating film and preparation method thereof Download PDF

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Publication number
CN104669712A
CN104669712A CN201510108012.0A CN201510108012A CN104669712A CN 104669712 A CN104669712 A CN 104669712A CN 201510108012 A CN201510108012 A CN 201510108012A CN 104669712 A CN104669712 A CN 104669712A
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plated film
film
layer
thermal isolation
alloy
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CN104669712B (en
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谈琦
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Qingdao Jiuyue New Material Technology Co.,Ltd.
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Sichuan Ya Li Supermembrane Science And Technology Ltd
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Abstract

The invention relates to a Ag alloy heat-insulating film and a preparation method thereof. The heat-insulating film comprises a base material PET (Polyethylene Glycol Terephthalate), a first NiCr film coating layer, a second Ag alloy film coating layer, and a third NiCr film coating layer. The preparation method for the heat-insulating film comprises the following steps: on a reel-to-reel flexible magnetron sputtering coating machine, when the base material PET is rotated along with a film coating roller, plating NiCr, Ag alloy and NiCr three film layers on the other side of the base material PET through film coating areas of different targets. The Ag alloy heat-insulating film disclosed by the invention has the advantages of being high in visible light transmission, high in infrared ray resistance, good in weather resistance, high in production efficiency, low in cost and the like, so that the application field of the heat-insulating film is widened, the market area is enlarged, and development of the heat insulating film towards energy conservation and environment protection direction is promoted.

Description

A kind of Ag alloy thermal isolation film and preparation method thereof
Technical field
The invention belongs to building and automobile adhesive film field, be specifically related to a kind of Ag alloy thermal isolation film with optical electivity permeability and preparation method thereof.
Background technology
Along with the proposition of the development of science and technology, the raising day by day of living standards of the people and " low-carbon (LC) life " idea, more and more higher to the performance requirement of thermal isolation film, demand is also progressively increasing.Current thermal isolation film has been widely used on the cladding glass of heavy construction and the glass pane of automobile.Utilize and can greatly reduce air-conditioning expense on the cladding glass of heavy construction, make the outward appearance of building have color attractive in appearance.Current most automotive glazing all posts thermal isolation film, and thermal isolation film reduces the injury of ultraviolet to human body and Che Nei ornaments, slows down the aging of car facilities, reduce the temperature of environment inside car, improve the environment by bus of driver and crew, also reduce the oil consumption of automobile simultaneously, save and use car cost.With regard to the development trend of thermal isolation film product, will have high visible light transmissivity while the heat-proof quality had, what can realize this requirement at present has noble metal and TiO 2or the multilayer complex films of the deielectric-coating such as ITO, but due to TiO 2sedimentation rate Deng deielectric-coating is very low, and namely production efficiency promote very much by low price very high being unfavorable for.The visible light transmissivity high with regard to general metal film and high heat-proof quality are conflicting, by suitable Method and process precious metals ag film can realize in varying degrees visible light transmissivity high while have good heat-proof quality, but there is the weatherability problems such as oxidizable and sulfuration in metal A g film.The present invention has good weatherability by the preparation of suitable technological process control, heat-proof quality is good and the Ag alloy thermal isolation film that visible light transmissivity is higher.
Summary of the invention
The object of the invention is to the market demand for current thermal isolation film, a kind of Ag alloy thermal isolation film with optical electivity permeability is provided, this thermal isolation film has that visible light transmissivity is high, infrared ray intercept high, production efficiency is high, low cost and other advantages, thus greatly increase the application of thermal isolation film, expand market scope, promote the industrialization of thermal isolation film.
Invention further provides a kind of preparation method of above-mentioned Ag alloy thermal isolation film, the Ag alloy thermal isolation film of nanoscale, size uniform can be obtained by this preparation method.
For achieving the above object, technical scheme of the present invention is as follows: continuously nickel plating evanohm (NiCr), yellow gold (AgCu) and nichrome (NiCr) trilamellar membrane successively on base material PET.
Further, Ag alloy thermal isolation film as above, wherein, the thickness of base material PET is 13 ~ 100 μm; The thickness of ground floor plated film nickel-chrome alloy layer is 0.2 ~ 3nm; The thickness of second layer plated film yellow gold layer is 5 ~ 15nm; The thickness of third layer plated film nickel-chrome alloy layer is 0.2 ~ 3nm.
Further, Ag alloy thermal isolation film as above, wherein, the weight percentage of ground floor plated film nichrome is: Ni80%Cr20%; The weight percentage of second layer plated film yellow gold is: Ag (90 ~ 98) %Cu (2 ~ 10) %, is preferably Ag92.5%Cu7.5%; The weight percentage of third layer plated film nichrome is: Ni80%Cr20%.
A kind of preparation method of Ag alloy thermal isolation film, the preparation of this thermal isolation film adopts the volume to volume magnetron sputtering coater being equipped with magnetron sputtering intermediate frequency twin target, until base material PET with film coating roller rotate through several air-tightness isolate good plated film district time, at another side continuously nickel plating evanohm (NiCr), yellow gold (AgCu) and nichrome (NiCr) trilamellar membrane successively of base material PET.
In plated film and reel system rotation process, what the coated surface on base material was in contact with it crosses roller can not have relative slip with pressure roller, because relative sliding can make coated surface scratch, and the oxidizable and sulfuration of scuffing place of coated surface, i.e. weatherability variation; The method adopted in the present invention is, all roller and pressure roller excessively are all equipped with self-aligning ball bearing, roller and pressure roller were all had and well rotates flexibility, ensure that the roller of crossing that base material is in contact with it does not have relative slip with pressure roller.The tension force of reel system can not be too large, and too conference is plated rete drawing crack for tension force, and namely weatherability is deteriorated.The tension force of reel system is regulated by rolling and the motor that unreels, the tension force of reel system is fine in order to what make base material and film coating roller fit, type variable in coating process after base material heated is as far as possible little, therefore the tension force of reel system can not be too little, in the present invention, rolling is the same with the Tensity size setting value unreeled, and setting range is 150-220N.
Further, the preparation method of Ag alloy thermal isolation film as above, wherein, the thickness of base material PET is 13 ~ 100 μm; The thickness of ground floor plated film nickel-chrome alloy layer is 0.2 ~ 3nm; The thickness of second layer plated film yellow gold layer is 5 ~ 15nm; The thickness of third layer plated film nickel-chrome alloy layer is 0.2 ~ 3nm.
Further, the preparation method of Ag alloy thermal isolation film as above, is coated with ground floor plated film nickel-chrome alloy layer by medium frequency magnetron sputtering nichrome twin target, and the power bracket of intermediate frequency power supply is 1.5 ~ 5kw; Be coated with second layer plated film yellow gold by medium frequency magnetron sputtering yellow gold twin target, the power bracket of intermediate frequency power supply is 10 ~ 30kw; Be coated with third layer plated film nickel-chrome alloy layer by medium frequency magnetron sputtering nichrome twin target, the power bracket of intermediate frequency power supply is 1.5 ~ 5kw.
Further, Ag alloy thermal isolation film as above, wherein, the weight percentage of ground floor plated film nichrome is: Ni80%Cr20%; The weight percentage of second layer plated film yellow gold is: Ag (90 ~ 98) %Cu (2 ~ 10) %, is preferably Ag92.5%Cu7.5%; The weight percentage of third layer plated film nichrome is: Ni80%Cr20%.
Further, in order to the Ag alloy thermal isolation film of obtained good weatherability, before plated film and in coating process, the cryogenic system of coating machine will run, unreeling district and each plated film district and will arrange deep cooling coil pipe at vacuum chamber, when cryogenic system runs, the temperature of deep cooling coil pipe is lower than subzero 120 DEG C, and vacuum chamber steam that is interior and base material releasing can be solidified on deep cooling coil pipe instantaneously, such first ensure that the vacuum needed for plated film, and second ensure that and do not have Vapor adsorption on film plating layer.
Beneficial effect of the present invention is as follows: flatness and the compactness on the surface of nichrome (NiCr) layer are all better than base material PET, yellow gold (AgCu) layer be coated with on the surface of nichrome (NiCr) layer, can increase yellow gold (AgCu) layer compactness and resistance to oxidation cure; Nichrome (NiCr) layer can play a protective role to yellow gold (AgCu) layer, increases resistance to oxidation cure.
The present invention obtains the silver-bearing copper rete with alloy phase by the mode of doping, and remaining silverskin has compared with high permeability at visible ray, have high reflectance infrared, namely has the advantage of better optical electivity permeability; Again by being coated with nichrome (NiCr) transition zone and protective layer, and be coated with the control of technique in process and obtain weatherability good Ag alloy thermal isolation film.
When winding speed one timing of base material, by regulating the power of each target to control the thickness of be coated with rete; Due to ground floor plated film and third layer plated film all thinner, the too little meeting of power of intermediate frequency power supply causes the electric discharge of target material surface uneven, the thickness of film plating layer is just uneven, transmitance and the color relation of gained thermal isolation film are uneven, so in order to ensure on the uniformity that target material surface discharges and base material be coated with the uniformity of film thickness, the power of intermediate frequency power supply can not be too little.
The thermal isolation film of gained of the present invention has the advantages such as visible light transmissivity is high, infrared ray obstruct is high, production efficiency high cost is low.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention has the Ag alloy thermal isolation film of optical electivity permeability.
In figure, 1 is base material PET, and 2 is ground floor nichrome (NiCr), and 3 is second layer yellow gold (AgCu), and 4 is third layer nichrome (NiCr).
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is further detailed explanation.
Ag alloy thermal isolation film structure provided by the present invention as shown in Figure 1, comprise base material PET 1, ground floor plated film nichrome (NiCr) 2, second layer plated film yellow gold (AgCu) 3 and third layer plated film nichrome (NiCr) 4, each layer characteristic is as follows:
Base material PET 1: be PETG, English name: polyethylene terephthalate.Thickness is 13 ~ 100 μm, has good heat resistance, heat resisting temperature >=120 DEG C.
Ground floor plated film nichrome (NiCr) 2: be coated with by medium frequency magnetron sputtering nichrome twin target, power supply is intermediate frequency power supply, being coated with thicknesses of layers is 0.2 ~ 3nm.Wherein, when rete is thicker, the more smooth densification in surface of gained nichrome film, the structure of the second layer plated film yellow gold (AgCu) be coated with in the above can be finer and close, more easily forms the yellow gold film plating layer of sheet crystal structure.But when nichrome thicknesses of layers is thicker, the visible light transmissivity of last gained thermal isolation film can be lower.Preferably, ground floor plated film nichrome thicknesses of layers is 0.2 ~ 1.5nm.
Second layer plated film yellow gold (AgCu) 3: be coated with by medium frequency magnetron sputtering yellow gold twin target, power supply is intermediate frequency power supply, being coated with thicknesses of layers is 5 ~ 15nm.The Main Function of Copper-cladding Aluminum Bar silver forms the yellow gold rete with alloy phase, and silver-copper alloy film has good resistance to oxidation curability.The Main Function of yellow gold (AgCu) film make use of silverskin to have higher transmitance to visible ray, has higher reflectivity to infrared ray.Preferably, second layer plated film yellow gold thicknesses of layers is 5 ~ 12nm.
Third layer plated film nichrome (NiCr) 4: be coated with by medium frequency magnetron sputtering nichrome twin target, power supply is intermediate frequency power supply, being coated with thicknesses of layers is 0.2 ~ 3nm.The Main Function of this tunic is protection second layer plated film yellow gold layer, obtains the better thermal isolation film of weatherability.Preferably, third layer plated film nichrome thicknesses of layers is 0.2 ~ 1.5nm.
Invention further provides the preparation method of above-mentioned Ag alloy thermal isolation film, be specially: adopt MF reactive magnetron sputtering twin target technology at one side successive sedimentation ground floor nichrome 2, second layer yellow gold 3, the third layer nichrome 4 successively of base material PET 1.
During underway frequency reaction magnetocontrol sputtering twin target plated film, even in order to ensure thicknesses of layers, all adopt symmetrical left, center, right three road air feed and binary gas distribution technology to combine air feed in each plated film district.
Before plated film and in coating process, cryogenic system will run, and unreeling district and each plated film district and will arrange deep cooling coil pipe at vacuum chamber, when cryogenic system runs, the temperature of deep cooling coil pipe is lower than subzero 120 DEG C.
During underway frequency reaction magnetocontrol sputtering twin target plated film, in order to monitor the transmissivity of deposited solar film, reflectivity and color, online optical monitoring equipment Real-Time Monitoring is adopted to obtain spectrogram and the chromaticity diagram of thermal isolation film.In order to ensure the uniformity of gained film, online optical monitoring device adopts multi-point monitoring, namely on the direction of base material fabric width, is respectively evenly arranged 3 control points.
The present invention adopts winding magnetron sputtering many targets coating machine in concrete enforcement, concrete technology parameter as shown in the following chart:
Note: the power of what the sputtering power in table referred to is exactly intermediate frequency power supply.
Concrete winding magnetron sputtering membrane process is: winding magnetron sputtering coater is primarily of vacuum system, reel system, cryogenic system, intermediate frequency twin target and intermediate frequency power supply composition, and wherein reel system forms with rolling by unreeling.The purity of film plating layer and quality in order to ensure, the background vacuum unreeling district and plated film district all will lower than 3.0x10 -3pa, controls by flowmeter the sputter gas Ar feeding 180sccm in each plated film district.When the winding speed certain (winding speed of base material can adjust within the scope of 0 ~ 50m/min) of base material, adjusted the thickness of every one deck plated film by the power of the intermediate frequency power supply adjusting each twin target.
Embodiment 1
Choose the base material PET that thickness is 100 μm, adopt the volume to volume magnetron sputtering coater being equipped with magnetron sputtering intermediate frequency twin target, until base material PET with film coating roller rotate through several air-tightness isolate good plated film district time, plate at its another side nichrome (Ni80%Cr20%) trilamellar membrane that thickness is the nichrome (Ni80%Cr20%) of 0.2nm, thickness is 5nm yellow gold (Ag92.5%Cu7.5%) and thickness are 0.2nm successively continuously, obtain Ag alloy thermal isolation film.
Adopt winding magnetron sputtering many targets coating machine in the present embodiment, concrete technology parameter as shown in the following chart:
Embodiment 2
Choose the base material PET that thickness is 13 μm, adopt the volume to volume magnetron sputtering coater being equipped with magnetron sputtering intermediate frequency twin target, until base material PET with film coating roller rotate through several air-tightness isolate good plated film district time, plate at its another side nichrome (Ni80%Cr20%) trilamellar membrane that thickness is the nichrome (Ni80%Cr20%) of 3nm, thickness is 15nm yellow gold (Ag92.5%Cu7.5%) and thickness are 3nm successively continuously, obtain Ag alloy thermal isolation film.
Adopt winding magnetron sputtering many targets coating machine in the present embodiment, concrete technology parameter as shown in the following chart:
Embodiment 3
Choose the base material PET that thickness is 80 μm, adopt the volume to volume magnetron sputtering coater being equipped with magnetron sputtering intermediate frequency twin target, until base material PET with film coating roller rotate through several air-tightness isolate good plated film district time, plate at its another side nichrome (Ni80%Cr20%) trilamellar membrane that thickness is the nichrome (Ni80%Cr20%) of 1nm, thickness is 8nm yellow gold (Ag92.5%Cu7.5%) and thickness are 1nm successively continuously, obtain Ag alloy thermal isolation film.
Adopt winding magnetron sputtering many targets coating machine in the present embodiment, concrete technology parameter as shown in the following chart:
Embodiment 4
Choose the base material PET that thickness is 50 μm, adopt the volume to volume magnetron sputtering coater being equipped with magnetron sputtering intermediate frequency twin target, until base material PET with film coating roller rotate through several air-tightness isolate good plated film district time, plate at its another side nichrome (Ni80%Cr20%) trilamellar membrane that thickness is the nichrome (Ni80%Cr20%) of 1.5nm, thickness is 12nm yellow gold (Ag92.5%Cu7.5%) and thickness are 1.5nm successively continuously, obtain Ag alloy thermal isolation film.
Adopt winding magnetron sputtering many targets coating machine in the present embodiment, concrete technology parameter as shown in the following chart:
As can be seen from above-described embodiment 1 ~ 4, can be controlled 20 ~ 75% by the visible light transmissivity of Ag alloy thermal isolation film provided by the invention, particularly when the structure of Ag alloy thermal isolation film is NiCr (0.2 ~ 1.5nm)/AgCu (5 ~ 12nm)/NiCr (0.2 ~ 1.5nm), its visible light transmissivity can control 50 ~ 75%, and it is very low to the infrared light transmission of this structure, less than 10%, have that visible light transmissivity is high, infrared ray intercepts high advantage, there are extraordinary application prospect and market prospects.
Those of ordinary skill in the art will appreciate that, embodiment described here is to help reader understanding's principle of the present invention, should be understood to that protection scope of the present invention is not limited to so special statement and embodiment.Those of ordinary skill in the art can make various other various concrete distortion and combination of not departing from essence of the present invention according to these technology enlightenment disclosed by the invention, and these distortion and combination are still in protection scope of the present invention.

Claims (10)

1. an Ag alloy thermal isolation film, is characterized in that: continuously nickel plating evanohm (NiCr), yellow gold (AgCu) and nichrome (NiCr) trilamellar membrane successively on base material PET.
2. a kind of Ag alloy thermal isolation film as claimed in claim 1, is characterized in that: the thickness of base material PET is 13 ~ 100 μm; The thickness of ground floor plated film nickel-chrome alloy layer is 0.2 ~ 3nm; The thickness of second layer plated film yellow gold layer is 5 ~ 15nm; The thickness of third layer plated film nickel-chrome alloy layer is 0.2 ~ 3nm.
3. a kind of Ag alloy thermal isolation film as claimed in claim 2, is characterized in that: the weight percentage of ground floor plated film nichrome is: Ni80%Cr20%; The weight percentage of second layer plated film yellow gold is: Ag (90 ~ 98) %Cu (2 ~ 10) %; The weight percentage of third layer plated film nichrome is: Ni80%Cr20%.
4. a kind of Ag alloy thermal isolation film as claimed in claim 3, is characterized in that: the weight percentage of yellow gold is: Ag92.5%Cu7.5%.
5. the preparation method of the arbitrary described Ag alloy thermal isolation film of claim 1-4, it is characterized in that: adopt the volume to volume magnetron sputtering coater being equipped with magnetron sputtering intermediate frequency twin target, until base material PET with film coating roller rotate through several air-tightness isolate good plated film district time, at another side continuously nickel plating evanohm (NiCr), yellow gold (AgCu) and nichrome (NiCr) trilamellar membrane successively of base material PET.
6. the preparation method of a kind of Ag alloy thermal isolation film as claimed in claim 5, is characterized in that: the thickness of base material PET is 13 ~ 100 μm; The thickness of ground floor plated film nickel-chrome alloy layer is 0.2 ~ 3nm; The thickness of second layer plated film yellow gold layer is 5 ~ 15nm; The thickness of third layer plated film nickel-chrome alloy layer is 0.2 ~ 3nm.
7. the preparation method of a kind of Ag alloy thermal isolation film as claimed in claim 6, is characterized in that: be coated with ground floor plated film nickel-chrome alloy layer by medium frequency magnetron sputtering nichrome twin target, and the power bracket of intermediate frequency power supply is 1.5 ~ 5kw; Be coated with second layer plated film yellow gold by medium frequency magnetron sputtering yellow gold twin target, the power bracket of intermediate frequency power supply is 10 ~ 30kw; Be coated with third layer plated film nickel-chrome alloy layer by medium frequency magnetron sputtering nichrome twin target, the power bracket of intermediate frequency power supply is 1.5 ~ 5kw.
8. the preparation method of a kind of Ag alloy thermal isolation film as described in as arbitrary in claim 5-7, is characterized in that: the weight percentage of described ground floor plated film nichrome is: Ni80%Cr20%; The weight percentage of second layer plated film yellow gold is: Ag (90 ~ 98) %Cu (2 ~ 10) %; The weight percentage of third layer plated film nichrome is: Ni80%Cr20%.
9. the preparation method of a kind of Ag alloy thermal isolation film as claimed in claim 8, is characterized in that: the weight percentage of yellow gold is: Ag92.5%Cu7.5%.
10. the preparation method of a kind of Ag alloy thermal isolation film as described in as arbitrary in claim 5-7, it is characterized in that: the cryogenic system running coating machine before plated film and in coating process, unreeling district and each plated film district and will arrange deep cooling coil pipe at vacuum chamber, when cryogenic system runs, the temperature of deep cooling coil pipe is lower than subzero 120 DEG C.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110144559A (en) * 2019-05-17 2019-08-20 中信戴卡股份有限公司 A kind of metal surface protection layer and preparation method thereof
US11072853B2 (en) 2018-03-21 2021-07-27 Citic Dicastal Co., Ltd High-ductility periodic variable alloy protective film and forming method thereof
CN114774870A (en) * 2022-04-19 2022-07-22 深圳格致黄金科技有限公司 Preparation process of new alloy/silver film coating material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474902A (en) * 2009-01-16 2009-07-08 中山市万丰胶粘电子有限公司 Heat-insulating film
CN203228452U (en) * 2013-05-07 2013-10-09 核工业西南物理研究院 Durable thermal insulation membrane structure and coatings
JP2014218042A (en) * 2013-05-10 2014-11-20 小川 倉一 Transparent heat insulation sheet and method for producing the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474902A (en) * 2009-01-16 2009-07-08 中山市万丰胶粘电子有限公司 Heat-insulating film
CN203228452U (en) * 2013-05-07 2013-10-09 核工业西南物理研究院 Durable thermal insulation membrane structure and coatings
JP2014218042A (en) * 2013-05-10 2014-11-20 小川 倉一 Transparent heat insulation sheet and method for producing the same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11072853B2 (en) 2018-03-21 2021-07-27 Citic Dicastal Co., Ltd High-ductility periodic variable alloy protective film and forming method thereof
CN110144559A (en) * 2019-05-17 2019-08-20 中信戴卡股份有限公司 A kind of metal surface protection layer and preparation method thereof
CN114774870A (en) * 2022-04-19 2022-07-22 深圳格致黄金科技有限公司 Preparation process of new alloy/silver film coating material

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