CN103395239A - Low-radiation thin film with silicon-aluminum nitride medium layer and preparation technology thereof - Google Patents
Low-radiation thin film with silicon-aluminum nitride medium layer and preparation technology thereof Download PDFInfo
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- CN103395239A CN103395239A CN2013102853860A CN201310285386A CN103395239A CN 103395239 A CN103395239 A CN 103395239A CN 2013102853860 A CN2013102853860 A CN 2013102853860A CN 201310285386 A CN201310285386 A CN 201310285386A CN 103395239 A CN103395239 A CN 103395239A
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Abstract
The invention discloses a low-radiation thin film with a silicon-aluminum nitride medium layer and a preparation technology thereof and belongs to the technical field of functional thin films. The low-radiation thin film is produced by using a magnetron sputtering method and comprises the following film layer structures of a tantalum transition layer, a silver layer and the silicon-aluminum nitride medium layer from a substrate to the top. The film layer is high in visible light transmittance, low in infrared radiation rate and long in service life. The preparation technology disclosed by the invention is simple, convenient to operate and low in production cost, has an extremely good industrial application prospect and can be widely applied to industries of energy-saving building glass, automobile glass and the like; the glass heat loss is reduced, and the energy consumption spent on controlling the room temperature is reduced.
Description
Technical field
The invention belongs to the function film technical field, be specifically related to a kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof.
Background technology
Low emissivity glass refers to that surface has been coated with the coated glass of low radiation film, low radiation film adopts silver as infrared-reflecting layers usually, can well stop thermal-radiating seeing through, be widely used in recent years the fields such as building, automobile, play good energy-saving effect.
Generally with magnetron sputtering method, prepared by off-line low radiation film commonly used.Because silver layer can cause low, the reflective height of light transmission, and very easily be corroded and be subject to mechanical wear, so need on silver layer, be coated with media coating, its effect is to improve visible light transmissivity by optical interference, reduce reflectivity, improve appearance luster, improve simultaneously its chemical resistance and anti-mechanical wear performance.Interlayer between silver layer and substrate base often can also play the effect that increases Interface adhesive strength, improves the silver layer membrance casting condition.
Common single silver layer low-radiation film has two kinds of structures.A kind of is the sandwich structure of dielectric layer/silver layer/dielectric layer.The Chinese patent that is 201110049715.2 as application number discloses a kind of low radiation coated glass, and wherein the low radiation film structure is Ta
2O
5/ Ag/Ta
2O
5.Dielectric layer is by oxide Ta
2O
5Form, in using the reactive magnetron sputtering method preparation process, the silver that is in oxidizing atmosphere can be oxidized, in addition, at high temperature its inner oxygen also can carry out oxidation to silver layer, thereby its infrared transmittivity is raise and the visible light transmissivity reduction, low radiation effect variation.Another kind is the class sandwich structure of combination of media layer/silver layer/combination of media layer.The Chinese patent that is 201110381757.6 as application number discloses a kind of low radiation coated glass, and wherein the low radiation film structure is NbO
x/ ZnAlO
x/ Ag/ZnAlO
x/ ZnSnO
3/ Si
3N
4Low radiation coated glass, wherein, the first dielectric layer is NbO
x, Nb is noble metal, has increased undoubtedly the cost of raw material; Second medium layer and the 3rd dielectric layer are oxide ZnAlO
x, have equally the oxidized problem of silver layer, thereby its infrared transmittivity raise and the visible light transmissivity reduction, low radiation effect variation.Therefore, often there is following shortcoming in existing low radiation film: (1) is not suitable for using the reactive magnetron sputtering method preparation; (2) rete is more, and complex structure causes complex manufacturing, and production efficiency is low; (3) use noble metal, production cost increases.
Summary of the invention
The objective of the invention is the deficiency for existing low radiation film, a kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof are provided, be characterized in: (1) adopts the preparation of reactive magnetron sputtering method room temperature, avoid the oxidation of silver layer, utilized its low emissivity glass for preparing under higher temperature, to use; (2) this low radiation film is the trilamellar membrane structure, and is simple in structure, simplified production technology, improved production efficiency; (3) use conventional raw materials, greatly reduce cost.In addition, this low radiation film visible light transmissivity is high, and infrared emittance is low, and color is Natural color.Transition zone tantalum used has wettability preferably to glass, has improved the growth conditions of silver layer, makes silverskin be two-dimensional growth, and silverskin is fine and close continuously, has reduced the film radiance; That the aluminium silicon nitride dielectric layer has is corrosion-resistant, resistance to oxidation, the advantage such as wear-resistant, makes low radiation film have long service life.
A kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, is characterized in that, from substrate base, up is followed successively by transition zone, functional layer, dielectric layer, and described transition zone is tantalum film, and described functional layer is silverskin, and described dielectric layer is aluminium silicon nitride.Film layer structure is the sandwich structure of tantalum transition zone/silver layer/aluminium silicon nitride dielectric layer.
The thickness of described transition zone tantalum film is 1.0～1.5nm, and the thickness of described function silver layer is 10～14nm, and the thickness of described outer aluminium silicon nitride dielectric layer is 55～65nm.
Described substrate base is glass substrate or macromolecular material substrate (PMMA or PC or PET or PMP).
The technical scheme that realizes the object of the invention is: a kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, use magnetic control sputtering device depositional coating structure on substrate base to be the low radiation film of tantalum transition zone/silver layer/aluminium silicon nitride dielectric layer.Its concrete steps are as follows:
(1) substrate pre-treatment
Watery hydrochloric acid, deionized water, the pH value that substrate base is 4～6 by the pH value successively is 8～10 sodium hydroxide solution, deionized water, alcohol, to clean glass substrate, removes the dirts such as its surface and oil contaminant incrustation, then 50～70 ℃ of dry for standby in baking oven.
(2) plated film
1) prepare
Carry out the plated film work early-stage preparations of magnetic control sputtering device.
2) put into substrate and target
1. put into target
By purity be 99.99% silico-aluminum target, purity, be that 99.99% tantalum metallic target and purity are that 99.99% silver metal target is put on coating machine sputtering chamber radio-frequency head target position.
2. put into substrate
Get (1) step clean dry substrate base glass or macromolecular material (PMMA or PC or PET or PMP), put on the sputtering chamber specimen holder, target position and sample interval are from being 8～12cm.
3) vacuumize
The (2)-2) after step completes, sputtering chamber is evacuated to 3.5 * 10
-3Below Pa.
4) ventilate and regulate its stagnation pressure
The (2)-3) after step completes, to passing into purity in the sputtering chamber of coating machine, be 99.99% sputter gas Ar, and regulate stagnation pressure to 0.8～1.2Pa.
5) sputter
The (2)-4) after step completes, to regulate radio-frequency power and make tantalum target build-up of luminance, adjustments operating pressure is 1Pa, opens and rotates.The first pre-sputtering 1min of tantalum target before plated film, to remove the target material surface pollutant.The tantalum target power output is adjusted into 40～60W, opens baffle plate, starts plated film, and substrate temperature is room temperature.Prepare the transition zone tantalum film, plated film time 25～35s, thicknesses of layers are 1～1.5nm.Close radio frequency, open silver-colored target radio frequency, regulate and make its build-up of luminance, silver-colored target power output is adjusted into 80～120W, prepares silverskin, and plated film time 40～50s, thicknesses of layers are 10～14nm.Close silver-colored target radio frequency, open silico-aluminum target radio frequency, adjusting makes its build-up of luminance, it is 99.99% reaction nitrogen that the backward vacuum chamber of build-up of luminance passes into purity, and its flow-control is at 20～40sccm, and the adjustment operating pressure is 1Pa, the silico-aluminum target power output is adjusted into 60～100W, prepare the aluminium silicon nitride film, plated film time 120～150min, thicknesses of layers are 55～65nm.In whole coating process, operating pressure maintains 1Pa all the time.
(3) finish sputter
After (2) step completes, take out aluminium silicon nitride dielectric layer low radiation film sample.
After the present invention adopts technique scheme, mainly contain following effect:
(1) transition zone tantalum film and glass have wettability preferably, have improved the growth conditions of silver layer, make silverskin be two-dimensional growth, and silverskin is even, continuous, fine and close, have reduced the film radiance;
(2) adopt the aluminium silicon nitride dielectric layer, effectively avoided existing medium of oxides layer low radiation film in using the reactive magnetron sputtering method preparation process, the oxidation of silver layer in oxidizing atmosphere, and under high temperature, use or the oxidation of silver layer while processing, the quality of product improved; Aluminium silicon nitride has wear-resistant, resistance to oxidation and decay resistance preferably, has extended the service life of low radiation film; Aluminium silicon nitride has higher thermal conductivity, and the rete in the time of can avoiding high-temperature process comes off;
(3) to have preparation technology simple in the present invention, and production cost is low, and (fee of material of whole film system is at 0.5 yuan/m
2In), be easy to apply;
(4) product of the present invention is compared with other products of the same type, the product that visible light transmissivity is identical or close, and product infrared emittance of the present invention is low; The product that infrared emittance is identical or close, product visible light transmissivity of the present invention is high.
The accompanying drawing explanation
Fig. 1 is the structural representation of the aluminium silicon nitride dielectric layer low radiation film prepared of example 1 of the present invention.
In figure, be followed successively by from the bottom up glass substrate, tantalum transition zone, silver layer, aluminium silicon nitride dielectric layer.
The specific embodiment
Below in conjunction with the specific embodiment, further illustrate the present invention.
Embodiment 1
A kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, its concrete steps are as follows:
(1) substrate pre-treatment
Watery hydrochloric acid, deionized water, the pH value that glass substrate is 5 by the pH value successively is 9 sodium hydroxide solution, deionized water, alcohol, to clean glass substrate, removes the dirts such as its surface and oil contaminant incrustation, then 60 ℃ of dry for standby in baking oven.
(2) plated film
1) prepare
Carry out the plated film work early-stage preparations of magnetic control sputtering device.
2) put into substrate and target
1. put into target
By purity be 99.99% silico-aluminum target, purity, be that 99.99% tantalum metallic target and purity are that 99.99% silver metal target is put on coating machine sputtering chamber radio-frequency head target position.
2. put into substrate
Get the clean dry glass substrate of (1) step, put on the sputtering chamber specimen holder, target position and sample interval are from being 10cm.
3) vacuumize
The (2)-2) after step completes, sputtering chamber is evacuated to 3.5 * 10
-3Below Pa.
4) ventilate and regulate its stagnation pressure
The (2)-3) after step completes, to passing into purity in the sputtering chamber of coating machine, be 99.99% sputter gas Ar, and regulate stagnation pressure 1.0Pa.
(5) sputter
The (2)-4) after step completes, to regulate radio-frequency power and make tantalum target build-up of luminance, adjustments operating pressure is 1Pa, opens and rotates.The first pre-sputtering 1min of tantalum target before plated film, to remove the target material surface pollutant.The tantalum target power output is adjusted into 50W, opens baffle plate, starts plated film, and substrate temperature is room temperature.Prepare the transition zone tantalum film, plated film time 30s, thicknesses of layers are 1.2nm.Close tantalum target radio frequency, open silver-colored target radio frequency, regulate and make its build-up of luminance.The silver target power output is adjusted into 100W, prepares silverskin, and plated film time 45s, thicknesses of layers are 12nm.Close silver-colored target radio frequency, open silico-aluminum target radio frequency, adjusting makes its build-up of luminance, it is 99.99% reaction nitrogen that the backward vacuum chamber of build-up of luminance passes into purity, and its flow-control is at 30sccm, and the adjustment operating pressure is 1Pa, the silico-aluminum target power output is adjusted into 80W, prepare the aluminium silicon nitride film, plated film time 135min, thicknesses of layers are 60nm.In whole coating process, operating pressure maintains 1Pa all the time.
(3) finish sputter
After (2) step completes, take out aluminium silicon nitride dielectric layer low radiation film sample.
Embodiment 2
A kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, with embodiment 1, wherein:
In (1) step, the pH value is that 6 watery hydrochloric acid, pH value are 8 sodium hydroxide solution, then 70 ℃ of dry for standby in baking oven.
The (2)-2)-2. in the step, target position and sample interval are from being 8cm.
The (2)-5) in step, tantalum target power output 60W, prepare the transition zone tantalum film, and plated film time 25s, thicknesses of layers are 1.0nm.The silver target power output is 120W, prepares silverskin, and plated film time 40s, thicknesses of layers are 10.4nm.The reaction nitrogen flow is controlled at 40sccm, and the silico-aluminum target power output is adjusted into 100W, prepares the aluminium silicon nitride film, and plated film time 120min, thicknesses of layers are 57nm.
Embodiment 3
A kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, with embodiment 1, wherein:
In (1) step, the pH value is that 4 watery hydrochloric acid, pH value are 10 sodium hydroxide solution, then 50 ℃ of dry for standby in baking oven.
The (2)-2)-2. in the step, target position and sample interval are from being 12cm.
The (2)-5) in step, tantalum target power output 40W, prepare the transition zone tantalum film, and plated film time 35s, thicknesses of layers are 1.4nm.The silver target power output is 80W, prepares silverskin, and plated film time 50s, thicknesses of layers are 13.4nm.The reaction nitrogen flow is controlled at 30sccm, and the silico-aluminum target power output is adjusted into 60W, prepares the aluminium silicon nitride film, and plated film time 150min, thicknesses of layers are 63nm.
Embodiment 4
A kind of aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, with embodiment 1, wherein:
In (1) step, substrate base is the PET substrate.
The (2)-2)-2. in the step, target position and sample interval are from being 9cm.
The (2)-5) in step, tantalum target power output 45W, prepare the transition zone tantalum film, and thicknesses of layers is 0.8nm.The silver target power output is 90W, prepares silverskin, and thicknesses of layers is 11.4nm.The silico-aluminum target power output is 90W, prepares the aluminium silicon nitride film, and plated film time 140min, thicknesses of layers are 59nm.
Result of the test
With the aluminium silicon nitride dielectric layer low radiation film that embodiment 1 prepares, its main performance is as follows:
The visible light transmittance rate of aluminium silicon nitride dielectric layer low radiation film glass reaches 86.2%, and infrared emittance is 0.061, has excellent low radiance; With reference to the method for inspection of product in GB/T5137.3-2002 to the decay resistance of hydrogen sulfide gas, record sample corrosion front and back visible light transmissivity and change less than 4%, have good decay resistance.
Claims (4)
1. an aluminium silicon nitride dielectric layer low radiation film and preparation technology thereof, is characterized in that film layer structure up is followed successively by the sandwich structure of tantalum transition zone/silver layer/aluminium silicon nitride dielectric layer from substrate base.
2. a kind of aluminium silicon nitride dielectric layer low radiation film according to claim 1 and preparation technology thereof, it is characterized in that: described tantalum transition region thickness is 1～1.5nm, and described silver thickness is 10～14nm, and described aluminium silicon nitride thickness of dielectric layers is 55～65nm.
3. a kind of aluminium silicon nitride dielectric layer low radiation film according to claim 1 and preparation technology thereof, it is characterized in that: described substrate base is glass substrate or macromolecular material (PMMA or PC or PET or PMP).
4. a kind of aluminium silicon nitride dielectric layer low radiation film according to claim 1 and preparation technology thereof, it is characterized in that: its preparation technology's concrete steps are as follows:
(1) substrate base pre-treatment
Watery hydrochloric acid, deionized water, the pH value that substrate base is 4～6 by the pH value successively is 8～10 sodium hydroxide solution, deionized water, alcohol, to clean substrate base, removes the dirts such as its surface and oil contaminant incrustation, then 50～70 ℃ of dry for standby in baking oven;
(2) plated film
Target position and sample interval are from being 8～12cm.Regulate tantalum target radio-frequency power and make tantalum target build-up of luminance, adjust tantalum target power output to 40～60W.Prepare the transition zone tantalum film, plated film time 25～35s, thicknesses of layers are 1.2nm.Close tantalum target radio frequency, open silver-colored target radio frequency, regulate and make its build-up of luminance, adjusting silver-colored target power output is to 80～120W, prepares silverskin, and plated film time 40～50s, thicknesses of layers are 10～14nm.Close silver-colored target radio frequency, open silico-aluminum target radio frequency, regulate and make its build-up of luminance, adjust silico-aluminum target power output to 60～100W.Prepare the aluminium silicon nitride dielectric layer, plated film time 120～150min, thicknesses of layers are 55～65nm.In whole coating process, operating pressure maintains 1.0Pa all the time, and substrate frame is rotated with 20rpm, at ambient temperature plated film.
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| CN108342705A (en) * | 2018-03-14 | 2018-07-31 | 南京理工大学 | The preparation method of Ta base high-temperature protection coatings with self-healing function |
| CN109338287A (en) * | 2018-08-15 | 2019-02-15 | 南京理工大学 | A kind of texturing Ta/Ag wide warm area self-lubricating coat in use and preparation method thereof |
| CN111575658A (en) * | 2020-05-22 | 2020-08-25 | 太原理工大学 | Polymer/silver-based low-radiation nano multilayer film and preparation method thereof |
| CN112679112A (en) * | 2020-12-11 | 2021-04-20 | 安徽凤阳玻璃有限公司 | Off-line high-transmittance clean-color low-radiation steel-coated glass and manufacturing method thereof |
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Application publication date: 20131120 |