CN103383155A - Ti-alloy nitride selective-absorption film system and preparation method thereof - Google Patents

Ti-alloy nitride selective-absorption film system and preparation method thereof Download PDF

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CN103383155A
CN103383155A CN2013102516104A CN201310251610A CN103383155A CN 103383155 A CN103383155 A CN 103383155A CN 2013102516104 A CN2013102516104 A CN 2013102516104A CN 201310251610 A CN201310251610 A CN 201310251610A CN 103383155 A CN103383155 A CN 103383155A
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tialn
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陆卫
王晓芳
俞立明
王少伟
陈飞良
刘星星
简明
陈效双
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Shanghai Institute of Technical Physics of CAS
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Abstract

The invention discloses a Ti-alloy nitride selective-absorption film system. The selective-absorption film system comprises a metal substrate and further comprises a Ti-alloy nitride selective-absorption film, an anti-reflection dielectric film and an SiO2 protective film which are deposited on the metal substrate in sequence. The selective-absorption film system provided by the invention is characterized in that the solar absorptivity is greater than 97%; the solar emissivity is smaller than 3%; both the photo-thermal conversion efficiency and the heat-collecting efficiency are high. Under the premise of keeping high absorptivity and low emissivity, the selective-absorption film can meet the requirements of diversification and individuation of photo-thermal products such as solar water heaters and solar air conditioners by adjusting the components of Ti alloy. The selective-absorption film system is simple in structure and free from oxygen deposition, and has the characteristics of simple preparation technology and using less target materials, so that the production efficiency is greatly improved; the industrial large-scale production cost is lowered. Therefore, the selective-absorption film system is of great significance for the development of the field of solar selective heat absorption films.

Description

Ti alloy nitride selective absorbing film system and preparation method thereof
Technical field
The present invention relates to the system design of solar thermal collector selective heat-absorbing film, specifically refer to a kind of coating process efficient that can greatly improve, absorb low radiation-selective absorbing film system based on the height of Ti alloy nitride.
Technical background
The solar energy thermal transition is that a kind of energy conversion efficiency and utilization rate are high and with low cost, solar energy that can extensively promote in the whole society utilizes mode.Current solar thermal utilization is the most active, and formed industry.The photo-thermal switching rate is fast, the thermal efficiency is high, daylighting area is large owing to having for flat plate collector, simple in structure, reliable, cost is suitable, also have the characteristics such as bearing capacity is strong, have and build a series of advantages such as perfect integrated combination, just in the field of energy utilization develop rapidly.The solar thermal collector of which kind of form and structure no matter, a core coating for selective absorption of sunlight spectrum that is used for absorbing solar radiation all will be arranged, this coating has high-absorbility at Visible-to-Near InfaRed wave band (0.3～2.5 μ m), the function film that has low-launch-rate at infrared band, be for solar thermal collector, improve the key of photo-thermal transformation efficiency.And for the heated body in a practical application, its heat radiation concentration of energy is in wavelength is the infrared range of spectrum of 3.0～30.0 μ m, in order to reduce heat loss, prevent that the shortwave energy that absorbs from falling with the radiation of long wave form again, will keep alap heat emission than (usually representing with ε) in the heat radiation wave band, and namely be equivalent to make object to keep alap absorptivity in the heat radiation wave band.In a word, to make exactly sorbent surface when absorbing solar radiation to greatest extent, reduce as far as possible its radiation heat loss.
The existing TXT coating of the selective heat-absorbing film that occurs in the market, black chromium, AlN/Al, NiCrNxOy, TiNxOy etc.Yet TXT coating is as absorbing film, and its absorptivity is the highest only has 92%, and emissivity is but up to 40%; Chromium plating film system because of its technical process contaminated environment, seldom uses; AlN/Al is eliminated owing to not using for a long time under antivacuum hot environment; The absorption films such as the NiCrNxOy of present more use, TiNxOy, its preparation process need to be considered two kinds of reacting gas nitrogen and oxygen simultaneously, and because the participation of oxygen makes technological parameter be difficult to control, and very strict to the seal request of equipment.The disclosed NiCrNxOy absorption film of China Patent Publication No. CN1584445A is after having done graded bedding to the NiCr tenor, and preferably absorptivity just reaches 92%, and minimum radiance is 0.1.The disclosed TiN of China Patent Publication No. CN101240944A and CN201196495Y xO yFilm is adding silica SiO 2After antireflective film, absorptivity can reach 96%, and emissivity needs the content of accuracy controlling nitrogen and oxygen lower than 4%., consider from extensive coating technique angle, wishing very much new explained hereafter film is these problems that solves for this reason.
Summary of the invention
The invention discloses a kind of Ti alloy nitride selective absorbing film is.Propose a kind of simple in structure, do not relate to the oxygen element deposition problems, have preparation technology simple, use target quantity few, that can greatly improve industrial production efficiency has high-absorbility, low-launch-rate and a solar selective heat-absorbing film system of the excellent properties such as weatherability is strong, long service life.
Film structure of the present invention as shown in Figure 1, take metal substrate 1 as substrate, the top that film ties up to metal substrate 1 is followed successively by from bottom to top: be coated on Ti alloy nitride film 2, antireflection layer 3, silica membrane 4 on metal substrate 1.Wherein:
Described metal substrate 1 is the Cu paillon foil, or Al paillon foil, or deposition one deck Cu film on Al, Ni, glass, stainless steel paillon foil, or the Ag film (to reduce the emissivity of absorbing film system, the heat conductivility of this metal substrate is excellent simultaneously) of the infrared high reflection of deposition one deck on Al, Ni, stainless steel, Cu paillon foil.Described Cu substrate thickness is in the 50-350nm scope, preferably in the 100-150nm scope; Described Ag film thickness is in the 8-20nm scope, preferably in the 10-15nm scope.
Described absorbing membranous layer 2 is Ti alloy nitride film, and thickness is in the 80-120nm scope, and 95-105nm preferably too thinly can reduce absorptivity, too thickly can increase emissivity again.
The material of described absorbing membranous layer 2 is TiAlN or TiSiN, or one or more in TiAlSiN.Wherein the atomic ratio of Ti, Al or Si, three kinds of elements of N is Ti:Al, Si:N=0.2～0.5:0.5～0.8:1.0, preferably Ti:Al, Si:N=0.3～0.4:0.6～0.7:1.0.The refractive index of described absorbing membranous layer Ti alloy nitride film 2 is free to control by the content of regulating Al, Si the transition of its pottery character from metallicity to class.Can be individual layer TiAlN or the TiSiN of one-component ratio, or TiAlSiN film, or each layer component is than the above-mentioned TiAlN of different multilayers or TiSiN, or one or more in the TiAlSiN material, or component is with the above-mentioned TiAlN of gradient thickness or TiSiN, or the graded films of one or more formation in the TiAlSiN material.
Described antireflective media coating 3 is Si3N4 or AlN or its combination, and thickness is preferably in the 25-35nm scope in the 20-50nm scope.Described Si 3N 4Rete is material very stable under a kind of superhard wear, high temperature, and the protective layer performance that is as film is very excellent, can greatly improve weatherability and the stability of absorbing film.Silicon nitride film layer has very low diffusion coefficient to oxygen, and stability is arranged preferably, and the silicon nitride film layer of sputtering sedimentation is very closely knit, smooth smooth and hardness is very high, and mobile ion is had very strong blocking capability, and good corrosion stability is arranged.Described AlN has that thermal conductivity is high, thermal coefficient of expansion is little, is good heat shock resistance material, and the characteristics such as hardness is large, fusing point is high, the ability of anti-molten metal attack is strong, dielectric properties are good the highlyest are stabilized to 2200 ℃.Room temperature strength is good, and the rising of intensity temperature descends slower.AlN has high reflectance in the infrared light district greater than 2500nm, can further reduce radiance.Film of the present invention system is combined as anti-reflection layer and protective layer with Si3N4 or AlN or its, can greatly improve weatherability and the stability of absorbing film, thereby improve the service life of heat collector.
Described protective film 4 is the SiO2 film, and its thickness is preferably in the 70-90nm scope in the 50nm-150nm scope.Described SiO2 rete is that surface ceramic is outside the pale of civilization except making film, can further reduce emissivity.
Absorbing film of the present invention is as absorbed layer, with Si with Ti alloy nitride film 3N 4Or AlN or its combination, SiO 2Film is as anti-reflection layer and protective layer.By the adjustable refractive index of material, realize good anti-reflection effect, improved the absorptivity of film system.
Absorbing film of the present invention is that following advantage is arranged:
1, absorbing film of the present invention be solar absorptance greater than 97%, emissivity has the high characteristics of photo-thermal conversion efficiency less than 3%, can be widely used in the heat collector of solar energy optical-thermal conversion.
2, absorbing film of the present invention ties up to and keeps under high-absorbility and low-launch-rate prerequisite, has simple in structurely, uses target quantity few, can greatly improve the advantage of industrial production efficiency.
3, absorbing film of the present invention is owing to having used Si very stable under superhard wear and high temperature 3N 4Or AlN or its combined material, than other published absorbing films, greatly improved weatherability and the stability of absorbing film, thus the service life of having improved heat collector.
4, material therefor with low cost in absorbing film of the present invention system, the preparation method is simple, can greatly reduce the cost of industrial mass production, and the development in solar selective heat-absorbing film field is had very important meaning.
Ti alloy nitride selective absorbing film disclosed by the invention is to be coated with continuously on the large-area metal substrate by industrialization magnetron sputtering preparation method, is specifically undertaken by following several steps:
(1) growth Ti alloy selective absorption film TiAlN or TiSiN on Cu substrate 1, or TiAlSiN film, thickness are in the 80-120nm scope, and 95-105nm preferably too thinly can reduce absorptivity, too thickly can increase emissivity again.Its sputtering target material can be TiAl or TiSi target, or the TiAlSi target, carries out reactive sputtering with nitrogen as reacting gas; Perhaps adopt TiAlN or TiSiN, or the ceramic target of TiAlSiN, directly carry out sputter coating.
(2) on absorbing membranous layer 2, growth antireflective dielectric layer 3, its sputtering target material can be Al or Si target, carries out reactive sputtering with nitrogen as reacting gas; Perhaps adopt TiAlN or TiSiN, or the ceramic target of TiAlSiN, directly carry out sputter coating.Thickness is preferably in the 25-35nm scope in the 20-50nm scope.
(3) deposition SiO2 protective film 4 on antireflection film layer 3, be surface ceramic deposition shields except making film, can further reduce emissivity.Its thickness is preferably in the 70-90nm scope in the 50nm-150nm scope, by regulating SiO 2The thickness of film further reduces reflection, increases film is absorptivity.Its sputtering target material can be the Si target, carries out reactive sputtering with oxygen as reacting gas; Perhaps adopt SiO 2Ceramic target directly carries out sputter coating.
Description of drawings
Accompanying drawing 1 is Ti alloy nitride selective absorbing film architecture schematic diagram of the present invention, wherein:
1 is metal substrate;
2 is Ti alloy nitride film;
3 is silicon nitride or aluminium nitride or its builtup film;
4 is silica membrane.
Accompanying drawing 2 is Cu substrate/TiAlN/Si of the present invention 3N 4/ SiO 2The reflectance spectrum curve of absorbing film system.
Accompanying drawing 3 is Cu substrate/TiSiN/Si of the present invention 3N 4/ SiO 2The reflectance spectrum curve of absorbing film system.
Accompanying drawing 4 is Cu substrate/Ag/TiAlN/AlN/SiO of the present invention 2The reflectance spectrum curve of absorbing film system.
The specific embodiment
For making content of the present invention, technical scheme and advantage clearer, below be embodiment with the Ti alloy nitride absorbing film of the present invention's preparation, by reference to the accompanying drawings the specific embodiment of the present invention is elaborated:
Multi-target magnetic control sputtering equipment sputtering sedimentation is all adopted in the preparation that Ti alloy nitride absorbing film of the present invention is, the plated film metal substrate must carry out strict cleaning and dry up operation.Vacuum chamber vacuumizes processing before being coated with each tunic, and back end vacuum is evacuated to 2 * 10 -3Pa is above is excellent; Then put target, namely should form luminous plasma in the plated film chamber, and form " runway " of light at target material surface.Target material surface is carried out pre-sputtering under certain power condition, in order to form clean sputtering surface.Carry out thin film sputtering growth under metal substrate is sent to target with certain speed this moment.
Embodiment 1:
Cu substrate/TiAlN/Si 3N 4/ SiO 2Absorbing film system and preparation method thereof.
This absorbing film is to be specially: Cu paper tinsel substrate/Ti 0.38Al 0.62N film (103nm)/Si 3N 4Film (27nm)/SiO 2Film (80nm).
Take the technological parameter of the present embodiment magnetron sputtering apparatus used as example, this absorbing film is that the concrete preparation condition of each tunic is as follows:
(1) at first, take the Cu paper tinsel as substrate, employing is target by the TiAlN pottery that predefined Ti, Al, three kinds of element atomic ratios of N sinter, and deposits one deck TiAlN film in the pure argon atmosphere on the Cu film, and during by the control reactive sputtering, the chien shih film thickness grows into 103nm.In the present embodiment target used, three kinds of element atomic ratios are Ti:Al:N=0.38:0.62:1.00, and sputtering power is 1kW, IF-FRE 30kHz, and the Ar throughput is 35sccm;
(2) at Ti 0.38Al 0.62On the N selective absorption film, growth Si 3N 4Antireflection film layer.Take Si as target, pass into N gas and prepare Si as reacting gas 3N 4Film, reactive sputtering power 1kW, IF-FRE 30kHz, Ar throughput 80sccm, N throughput 40sccm, during by the control reactive sputtering, the chien shih film thickness grows into 27nm;
(3) at Si 3N 4Antireflection film layer growth protecting layer SiO 2Film continues take Si as target, passes into O gas and prepares SiO as reacting gas 2Film, reactive sputtering power 1kW, IF-FRE 40kHz, Ar throughput 200sccm, O throughput 20sccm, during by the control reactive sputtering, the chien shih film thickness grows into 54nm.
Just can finally complete the preparation of Ti alloy nitride solar selective heat-absorbing film through 3 cavitys.This film ties up to preparation process only needs Ti 0.38Al 0.62Two kinds of targets of N and Si, with low cost.
This film be reflectance spectrum as shown in Figure 2, the technical indicator of this film system is as follows:
The absorptivity of testing this film system according to GB GB/T6424-2007 and GB/T4271-2007 reaches 97.3%, emissivity 3.5%.
Embodiment 2:
Cu substrate/TiSiN/Si 3N 4/ SiO 2Absorbing film system and preparation method thereof.
This absorbing film is to be specially: Cu paper tinsel substrate/Ti 0.4Si 0.6N film (96nm)/Si 3N 4Film (30nm)/SiO 2Film (88nm).
Take the technological parameter of the present embodiment magnetron sputtering apparatus used as example, this absorbing film is that the concrete preparation condition of each tunic is as follows:
(1) at first, take the Cu paper tinsel as substrate, take TiN ceramic target and Si as target, carry out cosputtering under nitrogen and argon gas mixed atmosphere.The present embodiment sputtering power used is 1kW, IF-FRE 30kHz, and the Ar throughput is 60sccm, N throughput 35sccm.During by the control reactive sputtering, the chien shih film thickness grows into 96nm.
(2) at Ti 0.4Si 0.6On the N selective absorption film, growth Si 3N 4Antireflection film layer.Take Si as target, pass into N gas and prepare Si as reacting gas 3N 4Film, reactive sputtering power 1kW, IF-FRE 30kHz, Ar throughput 80sccm, N throughput 40sccm, during by the control reactive sputtering, the chien shih film thickness grows into 27nm;
(3) at Si 3N 4Antireflection film layer growth protecting layer SiO 2Film continues take Si as target, passes into O gas and prepares SiO as reacting gas 2Film, reactive sputtering power 1kW, IF-FRE 40kHz, Ar throughput 200sccm, O throughput 20sccm, during by the control reactive sputtering, the chien shih film thickness grows into 54nm.
Just can finally complete the preparation of Ti alloy nitride solar selective heat-absorbing film through 3 cavitys.This film ties up to preparation process only needs TiN and two kinds of targets of Si, with low cost.
This film be reflectance spectrum as shown in Figure 3, the technical indicator of this film system is as follows:
The absorptivity of testing this film system according to GB GB/T6424-2007 and GB/T4271-2007 reaches 97.0%, emissivity 3.2%.
Embodiment 3:
Cu substrate/Ag/TiAlN/AlN/SiO 2Absorbing film system and preparation method thereof.
This absorbing film is to be specially: Cu paper tinsel substrate/Ag film (10nm)/Ti 0.38Al 0.62N film (98nm)/AlN film (36nm)/SiO 2Film (54nm).
Take the technological parameter of the present embodiment magnetron sputtering apparatus used as example, this absorbing film is that the concrete preparation condition of each tunic is as follows:
(1) at first, take metal A g as target, the infrared high reflection Ag film of plating one deck 10nm on Cu paper tinsel substrate;
(2) on the Ag film, adopt the TiAlN pottery that sinters by predefined Ti, Al, three kinds of element atomic ratios of N to be target, deposition one deck TiAlN film in the pure argon atmosphere, during by the control reactive sputtering, the chien shih film thickness grows into 98nm.In the present embodiment target used, three kinds of element atomic ratios are Ti:Al:N=0.38:0.62:1.00, and sputtering power is 1kW, IF-FRE 30kHz, and the Ar throughput is 35sccm;
(3) at Ti 0.38Al 0.62On the N selective absorption film, the growing AIN antireflection film layer.Take the AlN pottery as target, directly carry out sputter and be coated with the AlN film.The present embodiment magnetron sputtering apparatus used, sputtering power are 2kW, IF-FRE 100kHz, and the Ar throughput is 100sccm, during by the control reactive sputtering, the chien shih film thickness grows into 36nm;
(4) on the AlN antireflection film layer, growth protecting layer SiO 2Film continues take Si as target, passes into O gas and prepares SiO as reacting gas 2Film, reactive sputtering power 1kW, IF-FRE 40kHz, Ar throughput 200sccm, O throughput 20sccm, during by the control reactive sputtering, the chien shih film thickness grows into 54nm.
This film is that emissivity can be low to moderate 2.5% because the Cu paper tinsel that has adopted plating Ag film is substrate.
This film be reflectance spectrum as shown in Figure 4, the technical indicator of this film system is as follows:
The absorptivity of testing this film system according to GB GB/T6424-2007 and GB/T4271-2007 reaches 96.2%, emissivity 2.5%.
Above-described embodiment is only in order to illustrate technological thought of the present invention and characteristics; its purpose is enable those skilled in the art to understand content of the present invention and implement according to this; scope of the present invention not only is confined to above-mentioned specific embodiment; be all equal variation or modifications of doing according to disclosed spirit, still be encompassed in protection scope of the present invention.

Claims (3)

1. a Ti alloy nitride solar selective absorbing film is, comprises metal substrate (1), Ti alloy nitride film (2), silicon nitride or aluminium nitride or its builtup film (3) and silica membrane (4), it is characterized in that:
Described film structure is: depositing Ti alloy nitride film (2), silicon nitride or aluminium nitride or its builtup film (3) and silica membrane (4) successively on metal substrate (1);
Described metal substrate (1) is the Cu paillon foil, Al paillon foil, or Al, Ni, glass or the stainless steel paillon foil of surface deposition one deck Cu film, or Al, Ni, stainless steel or the Cu paillon foil of the Ag film of the infrared high reflection of surface deposition one deck; The thickness range of described Cu film is 50-350nm, and its preferable range is 100-150nm; Described Ag film thickness scope is 8-20nm, and its preferable range is 10-15nm;
The thickness range of described Ti alloy nitride film (2) is 80-120nm, its preferable range is 95-105nm, film material is one or more in TiAlN, TiSiN and TiAlSiN, wherein the atomic ratio of Ti, Al or Si, three kinds of elements of N is Ti:Al, Si:N=0.2～0.5:0.5～0.8:1.0, and preferred atomic ratio is Ti:Al, Si:N=0.3～0.4:0.6～0.7:1.0;
Described silicon nitride or aluminium nitride or its builtup film (3) are Si 3N 4Or AlN or its combination, thickness range is 20-50nm, its preferable range is 25-35nm;
Described silica membrane (4) thickness range is 50nm-150nm, and its preferable range is in the 70-90nm scope.
2. a kind of Ti alloy nitride solar selective absorbing film according to claim 1 is it is characterized in that: the refractive index of described Ti alloy nitride film (2) is free to control by the content of regulating Al and Si the transition of its pottery character from metallicity to class; Described absorbing membranous layer (2) is individual layer TiAlN, the TiSiN of one-component ratio, or TiAlSiN film, or each layer component is than different multilayer TiAlN, TiSiN, or one or more in the TiAlSiN material, or component is with TiAlN, the TiSiN of gradient thickness or the graded films of one or more formation in the TiAlSiN material.
3. the preparation method that selective absorbing film as claimed in claim 1 is, is characterized in that comprising the following steps:
A is at Cu Grown Ti alloy selective absorption film TiAlN or TiSiN, or the TiAlSiN film, and its sputtering target material can be TiAl or TiSi target, or the TiAlSi target, carries out reactive sputtering with nitrogen as reacting gas; Perhaps adopt TiAlN or TiSiN, or the ceramic target of TiAlSiN, directly carry out sputter coating;
B on Ti alloy nitride film (2), grown silicon nitride or aluminium nitride or its builtup film (3), its sputtering target material can be Al or Si target, carries out reactive sputtering with nitrogen as reacting gas; Perhaps adopt TiAlN or TiSiN, or the ceramic target of TiAlSiN, directly carry out sputter coating;
C is at silicon nitride or aluminium nitride or the upper cvd silicon dioxide film (4) of its builtup film (3), and its sputtering target material can be the Si target, carries out reactive sputtering with oxygen as reacting gas; Perhaps adopt SiO 2Ceramic target directly carries out sputter coating.
CN2013102516104A 2013-06-21 2013-06-21 Ti-alloy nitride selective-absorption film system and preparation method thereof Pending CN103383155A (en)

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CN104691052A (en) * 2013-12-10 2015-06-10 财团法人工业技术研究院 Selective Absorption Film and Radiant Heat Recovery Generator
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CN107406974B (en) * 2015-01-19 2021-02-12 欧瑞康表面解决方案股份公司普费菲孔 Coating chamber for carrying out a vacuum-assisted coating method, heat shield and coating method
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CN107406974A (en) * 2015-01-19 2017-11-28 欧瑞康表面解决方案股份公司普费菲孔 For the coating chamber for the coating process for performing vacuum aided, thermal insulation board and coating process
WO2016116383A1 (en) * 2015-01-19 2016-07-28 Oerlikon Surface Solutions Ag, Pfäffikon Coating chamber for implementing of a vacuum-assisted coating process, heat shield, and coating process
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CN111158069A (en) * 2019-12-26 2020-05-15 中国人民解放军国防科技大学 Spectrum selective radiation infrared stealth material and preparation method thereof
CN112526663A (en) * 2020-11-04 2021-03-19 浙江大学 Atomic layer deposition-based absorption film and manufacturing method thereof
CN113774325A (en) * 2021-08-17 2021-12-10 湖北久之洋红外系统股份有限公司 Anti-dust high-hardness multispectral aluminum nitride film system and preparation method thereof
CN115113305A (en) * 2022-08-01 2022-09-27 蓝思科技（长沙）有限公司 Antireflection film and preparation method and application thereof
WO2024027645A1 (en) * 2022-08-01 2024-02-08 蓝思科技（长沙）有限公司 Anti-reflection film, and preparation method therefor and application thereof

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Application publication date: 20131106