CN106403329A - High-temperature solar selective absorbing coating and preparation method thereof - Google Patents
High-temperature solar selective absorbing coating and preparation method thereof Download PDFInfo
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- CN106403329A CN106403329A CN201610925415.9A CN201610925415A CN106403329A CN 106403329 A CN106403329 A CN 106403329A CN 201610925415 A CN201610925415 A CN 201610925415A CN 106403329 A CN106403329 A CN 106403329A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/225—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption for spectrally selective absorption
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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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
- C23C14/06—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
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
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- 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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/40—Solar thermal energy, e.g. solar towers
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Abstract
The invention provides a high-temperature solar selective absorbing coating and a preparation method thereof. According to the high-temperature solar selective absorbing coating, a metal material serves as a base material, and a metal reflection film layer, a diffusion stop film layer, an absorbing film layer and an antireflection film layer are arranged on the surface of the metal base material sequentially from inside to outside, wherein the absorbing film layer comprises four absorbing sublayers with metal contents decreasing in a gradient mode from inside to outside. The absorbing film layer comprises the four absorbing sublayers with the gradually varied metal contents, and the metal contents change in the gradient mode, so that diffusion of the coating is slight during the high-temperature work process, and the high temperature stability of the film layers is improved.
Description
Technical field
The present invention relates to technical field of solar utilization technique, more particularly, to a kind of low cost, the high temperature solar of high stability
Coating for selective absorption and preparation method thereof.
Background technology
Coating for selective absorption of sunlight spectrum is that have high-absorbility in Visible-to-Near InfaRed wave band, has in infrared band
The function film of low-launch-rate, is the key technology improving photo-thermal conversion efficiency for solar thermal collector.With solar heat
Using the continuous development of demand and technology, the range of application of solar energy heat collection pipe is from cryogenic applications（≤100℃）Xiang Zhongwen applies
(100 DEG C -350 DEG C) and high temperature apply (350 DEG C -500 DEG C) development, high in desalinization, solar electrical energy generation etc. constantly to meet
The use requirement of warm application.The coating for selective absorption also high high-temp stability to be possessed using for thermal-collecting tube, adapts to
The application conditions of hot environment.
High temperature solar energy selective absorption coating is mainly made up of four parts：Near base material is infrared high reflecting metal
Layer, be outwards followed successively by diffusion impervious layer, absorbed layer and anti-reflection layer, metal level select good conductive metal material for example aluminum, copper, silver,
The metals such as nickel, molybdenum, tungsten；If absorbed layer is made up of dried layer metal-dielectric composite material film, nano-sized metal particles are distributed on Jie
In material, its optical characteristics can control the intermediateness in metal and medium, and the absorption subgrade near metal back layer has
High refractive index and extinction coefficient, with each reduction absorbing tenor in subgrade, its refractive index and extinction coefficient are also gradually
Reduce；Anti-reflection layer adopts low-refraction and low extinction coefficient material, reduces the reflection to light as far as possible, obtains excellent selectivity
Absorbent properties.Study the continuous practice of high-performance, high stable, long-life high temperature solar energy selective absorbing coatings in people
In, employ the film structure of number of different types, such as SS-AlN/SS（Rustless steel aluminium nitride）、 W-Al2O3、Mo-
Al2O3、W-SiO2Deng coating, the structure of SS+ALN absorber coatings is made up of two ceramic metal Absorption of Medium subgrades, due to
The tenor difference of two ceramic metal Absorption of Medium subgrades is big, and the metal ingredient in coating easily spreads in high temperature, makes
Become to absorb subgrade change of component, coated optical performance decays, cause the aging of film layer and come off, lead to film layer to lose efficacy, limit
Make application in high temperature for this coating；Mo-Al2O3The feature of/Cu system is Mo-Al2O3Absorb subgrade and there is composition gradual change
The multiple sublayer structure of complexity, the bad control of complex process；Al2O3Layer adopts RF sputtering method, and radio-frequency (RF) sputtering equipment is complicated,
Sedimentation rate is low；W-Al2O3、W-SiO2Employ relatively valuable tungsten target, and flat target sputtering silicon target, the target of plane silicon target
Stock utilization is low, substantially increases the cost of film layer, hinders the development further of solar energy high temperature application.Therefore for too
Sun can high temperature utilize, need a kind of low cost, heat stability good, and the coating for selective absorption of simple process and preparation skill
Art.
Content of the invention
The present invention is directed to the deficiencies in the prior art, provides a kind of high temperature solar energy selective absorption coating and its preparation side
Method, the low cost of high temperature solar energy selective absorption coating, good stability, and preparation process is simple.
The present invention is achieved through the following technical solutions：There is provided a kind of high temperature solar energy selective absorption coating, with gold
Genus material is base material, on the surface of metal base, includes successively from the inside to the outside：Metallic reflection film layer, diffusion barrier film layer, absorption
Film layer and antireflective coating；Wherein, described absorbing membranous layer includes four absorption subgrades that tenor reduces from the inside to the outside in gradient.
Described metal base can be the metal material that stainless steel tube, carbon steel pipe etc. have Thermal conductivity.
Described absorbing membranous layer includes four absorption subgrades of tenor gradual change, and its tenor changes in gradient, makes
Its diffusing phenomenon in hot operation is very slight, improves the stability in high temperature for the film layer.
Preferably, described absorbing membranous layer be nickel oxide aluminum absorbing membranous layer, described absorbing membranous layer include tenor by interior extremely
The outer four nickel oxide aluminum reducing in gradient absorb subgrade.
Nickel aluminium element is introduced metallic reflection film layer by the present invention, and is sputtered by vacuum response, is allowed to generation and has well
The NiAlN selective absorption film of absorbability.By the use of the excellent antioxygenic property of Ni so as to as the medium in metal medium
Component, improves the resistance to elevated temperatures of film layer.
Preferably, described antireflective coating is SiO2-Al2O3Double anti-reflection films.
The present invention is in outermost SiO2A small amount of aluminum is introduced in antireflective coating（10-20at%）, by Si-Al alloys target
Reactive magnetron sputtering, generates SiO2-Al2O3Double antireflection film layers, further increase the absorbent properties of film layer, strengthen this simultaneously
The hardness on invention membrane system surface and wearability.
Preferably, the thickness of described metallic reflection film layer is 80-100nm, and the thickness of described diffusion barrier film layer is 15-
25nm, in described absorbing membranous layer, the thickness of four absorption subgrades from the inside to the outside is respectively 35-40nm, 30-35 nm, 25-30
Nm, 20-25 nm, the thickness of described antireflective coating is 80-100nm.
The present invention also provides a kind of preparation method of high temperature solar energy selective absorption coating, for preparing above-mentioned high temperature
Solar selectively absorbing coating, methods described is applied to intermediate frequency and pulse direct current vacuum magnetron sputtering film plating machine equipment, described
Method is carried out in accordance with the following steps：
S101：Substrate pretreatment：By metal base（1）It is polished rear deionized water to rinse, then dry passivation, make metal
The surface of base material forms passivation layer；
S102：Preheating：The metal base processing in step S101 is placed in the vacuum interior of coater, makes described metal base
Then the indoor temperature of vacuum can be increased to 350-400 DEG C, be incubated 30- around the central rotation of vacuum chamber while rotation
60min；
S103：Being coated with of metallic reflection film layer：Nickel aluminum target is sputtered using direct current pulse power source, is coated with metal in metallic substrate surface
Reflective coating, until described film layer reaches required design thickness；Its coating process parameter is：Background vacuum is in 4.0*10- 3Below Pa, in the range of 160-200sccm, process pressure is 2.0*10 to the argon flow amount being passed through vacuum film coating chamber-1-2.5*10- 1Pa；In the range of 400-450V, in the range of 40-45A, the plated film time is 8-10 to electric current to the sputtering voltage of direct current pulse power source
Minute；
During plated film, vacuum interior is passed through argon, and direct current pulse power source connected by nickel aluminum target, then argon ionization, in the work of electromagnetic field
With under, argon ion bombardment target, target molecule deposition metallic substrate surface formed plated film.
S104：Being coated with of diffusion barrier film layer：Using twin aluminum target medium frequency reactive sputtering mode, implement reactive sputtering plating
Film, until described film layer reaches required design thickness；Its coating process parameter is：The argon flow amount being passed through vacuum film coating chamber exists
In the range of 100-120sccm, in the range of 55-65sccm, its process pressure is 3.0*10 to the flow of reacting gas nitrogen-1-
3.5*10-1Pa；, in the range of 420-440V, in the range of frequency 40-60KHZ, electric current is in 40-45A model for intermediate frequency power supply sputtering voltage
In enclosing, the plated film time is 1-3 minute；
During plated film, vacuum interior is first passed through argon, connects intermediate frequency power supply, in the presence of electromagnetic field, argon then to twin aluminum target
Pneumoelectric, from, argon ion bombardment target, makes twin aluminum target sputtering, is now passed through nitrogen at once, carries out reactive sputtering, make target molecule
It is deposited on metal tube surface with gas molecule chemical combination, form thin film.
S105：Being coated with of absorbing membranous layer：
S1051：The preparation of the first absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 70-80sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, wherein aluminum target voltage in the range of 400-420V,
Electric current is in the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is in the range of 500-550V, electric
In the range of 40-45A, the plated film time is 3-5 minute to stream；
During plated film, vacuum interior is first passed through argon, connects intermediate frequency power supply then to twin aluminum target, connects DC pulse to nickel aluminum target
Power supply, in the presence of electromagnetic field, argon ion bombardment nickel aluminum target and twin aluminum target, the target molecule deposition of nickel aluminum target is in Metal Substrate
Material surface forms plated film；Reacted during the sputtering of twin aluminum target sputtering with the nitrogen being passed through, make twin aluminum target target molecule and
Gas molecule chemical combination is deposited on metal tube surface, forms thin film.
S1052：The preparation of the second absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, directly
Reach required design thickness to described film layer；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 60-70sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, wherein aluminum target voltage in the range of 400-420V,
Electric current is in the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is in the range of 450-500V, electric
In the range of 35-40A, the plated film time is 4-6 minute to stream；
S1053：The preparation of the 3rd absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 50-60sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, wherein aluminum target voltage in the range of 400-420V,
Electric current is in the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is in the range of 400-450V, electric
In the range of 30-35A, the plated film time is 5-7 minute to stream；
S1054：The preparation of the 4th absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 40-50sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, wherein aluminum target voltage in the range of 400-420V,
Electric current is in the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is in the range of 350-400V, electric
In the range of 25-30A, the plated film time is 6-8 minute to stream；
S106：Being coated with of antireflective coating：Using sial target mid frequency sputtering plated film mode, implement reactive sputtering plated film, until described
Film layer reaches required design thickness；Its coating process parameter is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, oxygen flow in the range of 50-60sccm, intermediate frequency power supply frequency in the range of 40-60KHZ, technique vacuum
Spend for 3.0*10-1-3.5*10-1Pa, in the range of 500-550V, the plated film time is 15-20 minute to sial target voltage.
During plated film, vacuum interior is passed through argon, and intermediate frequency power supply connected by sial target, then argon ionization, in the work of electromagnetic field
With under, argon ion bombardment sial target, be passed through oxygen during the sputtering of sial target, carry out reactive sputtering, target molecule and gas molecule
Conjunction is deposited on metal tube surface, forms thin film.
In the method preparing high temperature solar energy selective absorption coating that the present invention provides, straight using mid frequency sputtering and pulse
Stream sputtering, compared with radio-frequency (RF) sputtering equipment simply it is easy to manipulate, the technology stability of film layer preparation is strengthened, and film performance obtains into one
Step is improved.Especially medium frequency reactive sputtering is coated with SiO2-Al2O3Antireflection film layer, using magnetron sputtering cylindrical target（Si-Al alloy
Target）, it is prevented effectively from the easy starting the arc of flat target and the problem that heat conduction is uneven, target utilization also carries significantly compared with flat target simultaneously
High.And expensive tungsten target in the present invention, is replaced with nickel alumin(i)um alloy target, silicon flat target, the target of cylindrical target is replaced with silico-aluminum cylindrical target
Material utilization rate is almost 2 times of flat target target utilization, greatly reduces the preparation cost of film layer.
Preferably, described aluminum target, nickel aluminum target and sial target are column magnetic control sputtering target, aluminum target, sial target and metal base
The distance between be held in the range of 15-25cm, the distance between nickel aluminum target and metal base are maintained in the range of 5-15cm.
Technical scheme provided in an embodiment of the present invention can comprise following beneficial effect：
The present invention provides a kind of high temperature solar energy selective absorption coating and preparation method thereof, and described high temperature solar energy selective is inhaled
Receive coating with metal material as base material, on the surface of metal base, include successively from the inside to the outside：Metallic reflection film layer, diffusion resistance
Gear film layer, absorbing membranous layer and antireflective coating；Wherein, described absorbing membranous layer includes four that tenor reduces from the inside to the outside in gradient
Individual absorption subgrade.Described absorbing membranous layer includes four absorption subgrades of tenor gradual change, and its tenor changes in gradient,
Make its diffusing phenomenon in hot operation very slight, improve the stability in high temperature for the film layer.
Brief description
For the clearer explanation embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Have technology description in required use accompanying drawing be briefly described it is clear that, to those skilled in the art, not
On the premise of paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is a kind of structural representation of high temperature solar energy selective absorption coating provided in an embodiment of the present invention.
Fig. 2 is that a kind of technique of the preparation method of high temperature solar energy selective absorption coating provided in an embodiment of the present invention sets
The structural representation of standby vacuum chamber.
Shown in figure：The structure of high temperature solar energy selective absorption coating is from inside to outside that metal base, metal are anti-successively
Penetrate film layer, diffusion barrier film layer, absorbing membranous layer, antireflective coating.
Specific embodiment
In order that those skilled in the art more fully understand the technical scheme in the present invention, real below in conjunction with the present invention
Apply the accompanying drawing in example, the enforcement it is clear that described is clearly and completely described to the technical scheme in the embodiment of the present invention
Example is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, art technology
The every other embodiment that personnel are obtained under the premise of not making creative work, all should belong to the protection model of the present invention
Enclose.
The present invention provides a kind of preparation method of high temperature solar energy selective absorption coating, the height described in following embodiments
Temperature solar coating for selective absorption all in this approach based on prepare.
Embodiment 1
The present embodiment provides a kind of preparation method of high temperature solar energy selective absorption coating, and methods described adopts intermediate frequency and pulse
Direct-current vacuum magnetron sputtering coater is process equipment, and the vacuum chamber structure of described plated film machine equipment is as shown in Fig. 2 described matrix
It is fixed on the edge of described vacuum chamber, can also be around the center rotation of vacuum chamber while described matrix itself can rotate
Turn, described aluminum target, nickel aluminum target and sial target are column magnetic control sputtering target, the distance between aluminum target, sial target and metal base are all
For 15cm, the distance between nickel aluminum target and metal base are 5cm.The magnetic field of column magnetic control sputtering target is arranged as unbalanced magnetic field,
Due to the diversity of unbalanced magnetic field, increase effective plated film area of magnetic controlled sputtering target；Simultaneously using orientation sputtering, target core is solid
Fixed, target pipe rotates, and magnetic direction, in the face of metal base, makes matrix immerse in the plasma, on the one hand, the atom sputtering out
Form thin film with particle deposition in matrix surface, on the other hand, plasma bombards matrix with certain energy, plays ion beam
The effect of assistant depositing, improves the quality of film layer.
Methods described is carried out as follows：
S101：Substrate pretreatment：Stainless steel tube matrix is polished rear deionized water rinse, then dries passivation, make not
The surface of rust steel pipe matrix forms passivation layer；
S102：Preheating：The stainless steel tube processing in step S101 matrix is placed in the vacuum interior of coater, matrix can be certainly
Then the indoor temperature of vacuum can be increased to 350 DEG C, be incubated 30min around the central rotation of vacuum chamber while body rotates；
S103：Being coated with of metallic reflection film layer：Nickel aluminum target is sputtered using direct current pulse power source, first passes through argon gas distribution pipe to true
It is passed through argon in empty room, connect direct current pulse power source then to nickel aluminum target, then argon ionization, in the presence of electromagnetic field, argon
Ion bom bardment nickel aluminum target, target molecule deposition forms plated film on stainless steel base surface, until film layer reaches required design
Thickness, in the process, also around the rotation of 360 degree of the center of vacuum chamber while 360 degree of rotations of stainless steel base itself, so that target
Material molecule can form plated film on the circumference of the indoor all stainless steel bases of vacuum, the stainless steel base in following step and
Identical motion is done in this step；Its coating process parameter is：Background vacuum is in 4.0*10-3Pa, is passed through vacuum film coating chamber
Argon flow amount is 160sccm, and process pressure is 2.0*10-1-1Pa；The sputtering voltage of direct current pulse power source is 400V, and electric current is
40A, the plated film time is 8min；
S104：Being coated with of diffusion barrier film layer：Using twin aluminum target medium frequency reactive sputtering mode, first pass through argon gas distribution pipe to
Vacuum interior is passed through argon, connects intermediate frequency power supply then to twin aluminum target, after the normal sputtering of twin aluminum target, immediately passes through nitrogen cloth
Trachea is passed through nitrogen to vacuum interior, carries out reactive sputtering, and target molecule and gas molecule chemical combination are deposited on metal tube surface, shape
Become thin film, until film layer reaches required design thickness；Its coating process parameter is：The argon being passed through vacuum film coating chamber is
100sccm, the flow of reacting gas nitrogen is 55sccm, and its process pressure is 3.0*10-1Pa；Intermediate frequency power supply sputtering voltage is
420V, frequency is 40KHZ, and electric current is 40A, and the plated film time is 1min；
S105：Being coated with of absorbing membranous layer：
S1051：The preparation of the first absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, logical first
Cross argon gas distribution pipe and be passed through argon to vacuum interior, connect direct current pulse power source then to nickel aluminum target, in connecting to twin aluminum target
Frequency power, then argon ionization, in the presence of electromagnetic field, argon ion bombardment nickel aluminum target and twin aluminum target, nickel aluminum target divides
Son is deposited on stainless steel base surface and forms plated film, after the normal sputtering of twin aluminum target, immediately passes through nitrogen gas distribution pipe to vacuum chamber
Inside it is passed through nitrogen, carry out reactive sputtering, target molecule and gas molecularization are closed and be deposited on metal tube surface, form thin film, until
Film layer reaches required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is 100sccm,
Nitrogen flow is 70sccm；Technique vacuum is 3.0*10-1Pa, is powered to twin aluminum target using intermediate frequency power supply, frequency is
40KHZ, wherein aluminum target voltage are 400V, and electric current is 40A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is
500V, electric current is 40A, and the plated film time is 3min；
S1052：The preparation of the second absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness, its film plating process is identical with above-mentioned steps S1051；The technological parameter of its plated film is：Logical
The argon flow amount entering vacuum film coating chamber is in the range of 100sccm, and nitrogen flow is 60sccm；Technique vacuum is in 3.0*10-1Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency is 40KHZ, wherein aluminum target voltage is 400V, electric current is 40A；Using direct current
The pulse power is powered to nickel aluminum target, and nickel aluminum target voltage is 450V, and electric current is 35A, and the plated film time is 4min；
S1053：The preparation of the 3rd absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness, film plating process is with step S1051；The technological parameter of its plated film is：It is passed through vacuum film coating chamber
Argon flow amount in 100sccm, nitrogen flow is 50sccm；Technique vacuum is 3.0*10-1Pa, is given twin using intermediate frequency power supply
Aluminum target is powered, and frequency is 40KHZ, and wherein aluminum target voltage is 400V, and electric current is 40A；Supplied to nickel aluminum target using direct current pulse power source
Electricity, nickel aluminum target voltage is 400V, and electric current is 30A, and the plated film time is 5min；
S1054：The preparation of the 4th absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness, the same S1051 of plating steps；The technological parameter of its plated film is：It is passed through the argon of vacuum film coating chamber
Throughput is 100sccm, and nitrogen flow is 40sccm；Technique vacuum is 3.0*10-1Pa, gives twin aluminum target using intermediate frequency power supply
Power supply, frequency is 40KHZ, and wherein aluminum target voltage is 400V, and electric current is 40A；Powered to nickel aluminum target using direct current pulse power source, nickel
Aluminum target voltage is 350V, and electric current is 25A, and the plated film time is 6min；
S106：Being coated with of antireflective coating：Using sial target mid frequency sputtering plated film mode, implement reactive sputtering plated film, first pass through
Argon gas distribution pipe is passed through argon to vacuum interior, connects intermediate frequency power supply then to sial target, after the normal sputtering of sial target, leads at once
Cross oxygen gas distribution pipe and be passed through oxygen to vacuum interior, carry out reactive sputtering, target molecule and gas molecule chemical combination are deposited on metal
Pipe surface, forms thin film, until described film layer reaches required design thickness；Its coating process parameter is：It is passed through vacuum coating
The argon flow amount of room is 100sccm, and oxygen flow is 50sccm, and intermediate frequency power supply frequency is 40KHZ, and technique vacuum is 3.0*
10-1Pa, the voltage of sial target is 500V, and the plated film time is 15min.
The high temperature solar energy selective absorption coating being obtained on the surface of stainless steel tube matrix using said method, its structure
As shown in figure 1, including successively from the inside to the outside on the surface of stainless steel tube matrix：Metallic reflection film layer, diffusion barrier film layer, absorption
Film layer and antireflective coating；Wherein, described absorbing membranous layer includes four absorption subgrades that tenor reduces from the inside to the outside in gradient,
The tenor of four absorption subgrades changes in gradient so as to the diffusing phenomenon in hot operation are very slight, improves film layer
Stability in high temperature.Described absorbing membranous layer is nickel oxide aluminum absorbing membranous layer, and nickel aluminium element is introduced metallic reflection film layer, and
Sputtered by vacuum response, be allowed to generate the NiAlN selective absorption film with good absorption ability.Using excellent the resisting of Ni
Oxidation susceptibility is so as to as the metal component in metal medium, improve the resistance to elevated temperatures of film layer.Described antireflective coating is
SiO2-Al2O3Anti-reflection film, in outermost SiO2A small amount of aluminum is introduced, by the magnetic control reaction of Si-Al alloys target in antireflective coating
Sputtering, generates SiO2-Al2O3Double antireflection film layers, further increase the absorbent properties of film layer, strengthen membrane system of the present invention simultaneously
The hardness on surface and wearability.
In the present embodiment, the thickness of described metallic reflection film layer is 80nm, and the thickness of described diffusion barrier film layer is 15nm,
In described absorbing membranous layer, the thickness of four absorption subgrades from the inside to the outside is respectively 35nm, 30nm, 25nm, 20nm, described anti-reflection
The thickness of film layer is 80nm.
Embodiment 2
The present embodiment provides a kind of preparation method of high temperature solar energy selective absorption coating, and methods described adopts intermediate frequency and pulse
Direct-current vacuum magnetron sputtering coater is process equipment, and the vacuum chamber structure of described plated film machine equipment is as shown in Fig. 2 described matrix
It is fixed on the edge of described vacuum chamber, can also be around the center rotation of vacuum chamber while described matrix itself can rotate
Turn, described aluminum target, nickel aluminum target and sial target are column magnetic control sputtering target, the distance between aluminum target, sial target and metal base are all
For 25cm, the distance between nickel aluminum target and metal base are 15cm.The magnetic field of column magnetic control sputtering target is arranged as unbalanced magnetic field,
Due to the diversity of unbalanced magnetic field, increase effective plated film area of magnetic controlled sputtering target；Simultaneously using orientation sputtering, target core is solid
Fixed, target pipe rotates, and magnetic direction, in the face of metal base, makes matrix immerse in the plasma, on the one hand, the atom sputtering out
Form thin film with particle deposition in matrix surface, on the other hand, plasma bombards matrix with certain energy, plays ion beam
The effect of assistant depositing, improves the quality of film layer.
Methods described is carried out as follows：
S101：Substrate pretreatment：Stainless steel tube matrix is polished rear deionized water rinse, then dries passivation, make not
The surface of rust steel pipe matrix forms passivation layer；
S102：Preheating：The stainless steel tube processing in step S101 matrix is placed in the vacuum interior of coater, then by vacuum
Indoor temperature is increased to 400 DEG C, is incubated 60min；
S103：Being coated with of metallic reflection film layer：Nickel aluminum target is sputtered using direct current pulse power source, first passes through argon gas distribution pipe to true
It is passed through argon in empty room, connect direct current pulse power source then to nickel aluminum target, then argon ionization, in the presence of electromagnetic field, argon
Ion bom bardment nickel aluminum target, target molecule deposition forms plated film on stainless steel base surface, until film layer reaches required design
Thickness, in the process, also around the rotation of 360 degree of the center of hollow chamber while 360 degree of rotations of stainless steel base itself, so that target
Material molecule can form plated film on the circumference of the indoor all stainless steel bases of vacuum, the stainless steel base in following step and
Identical motion is done in this step；Its coating process parameter is：Background vacuum is 2.0*10-3Pa, is passed through vacuum film coating chamber
Argon flow amount is 200sccm, and process pressure is 2.5*10-1Pa；The sputtering voltage of direct current pulse power source is 450V, and electric current is 45A,
The plated film time is 10min；
S104：Being coated with of diffusion barrier film layer：Using twin aluminum target medium frequency reactive sputtering mode, first pass through argon gas distribution pipe to
Vacuum interior is passed through argon, connects intermediate frequency power supply then to twin aluminum target, after the normal sputtering of twin aluminum target, immediately passes through nitrogen cloth
Trachea is passed through nitrogen to vacuum interior, carries out reactive sputtering, and target molecule and gas molecule chemical combination are deposited on metal tube surface, shape
Become thin film, until film layer reaches required design thickness；Its coating process parameter is：The argon flow amount being passed through vacuum film coating chamber is
120sccm, the flow of reacting gas nitrogen is 65sccm, and its process pressure is 3.5*10-1Pa；Intermediate frequency power supply sputtering voltage is
440V, frequency is 60KHZ, and electric current is 45A, and the plated film time is 3min；
S105：Being coated with of absorbing membranous layer：
S1051：The preparation of the first absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, logical first
Cross argon gas distribution pipe and be passed through argon to vacuum interior, connect direct current pulse power source then to nickel aluminum target, in connecting to twin aluminum target
Frequency power, then argon ionization, in the presence of electromagnetic field, argon ion bombardment nickel aluminum target and twin aluminum target, nickel aluminum target divides
Son is deposited on stainless steel base surface and forms plated film, after the normal sputtering of twin aluminum target, immediately passes through nitrogen gas distribution pipe to vacuum chamber
Inside it is passed through nitrogen, carry out reactive sputtering, target molecule and gas molecularization are closed and be deposited on metal tube surface, form thin film, until
Film layer reaches required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is 120sccm,
Nitrogen flow is 80sccm；Technique vacuum is 3.5*10-1Pa, is powered to twin aluminum target using intermediate frequency power supply, frequency is
60KHZ, wherein aluminum target voltage are 420V, and electric current is 45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is
550V, electric current is 45A, and the plated film time is 3min；
S1052：The preparation of the second absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness, its film plating process is identical with above-mentioned steps S1051；The technological parameter of its plated film is：Logical
The argon flow amount entering vacuum film coating chamber is in the range of 120sccm, and nitrogen flow is in the range of 70sccm；Technique vacuum is 3.5*
10-1Pa, is powered to twin aluminum target using intermediate frequency power supply, and frequency is 60KHZ, and wherein aluminum target voltage is 420V, and electric current is 45A；Adopt
Powered to nickel aluminum target with direct current pulse power source, nickel aluminum target voltage is 500V, electric current is 40A, the plated film time is 4min；
S1053：The preparation of the 3rd absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness, film plating process is with step S1051；The technological parameter of its plated film is：It is passed through vacuum film coating chamber
Argon flow amount 120sccm, nitrogen flow be 60sccm；Technique vacuum is 3.5*10-1Pa, is given twin using intermediate frequency power supply
Aluminum target is powered, and frequency is 60KHZ, and wherein aluminum target voltage is 420V, and electric current is 45A；Supplied to nickel aluminum target using direct current pulse power source
Electricity, nickel aluminum target voltage is 450V, and electric current is 35A, and the plated film time is 5min；
S1054：The preparation of the 4th absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness, film plating process is with step S1051；The technological parameter of its plated film is：It is passed through vacuum film coating chamber
Argon flow amount be 120sccm, nitrogen flow be 50sccm；Technique vacuum is 3.5*10-1Pa, is given twin using intermediate frequency power supply
Aluminum target is powered, and frequency is 60KHZ, and wherein aluminum target voltage is 420V, and electric current is 45A；Supplied to nickel aluminum target using direct current pulse power source
Electricity, nickel aluminum target voltage is 400V, and electric current is 30A, and the plated film time is 6min；
S106：Being coated with of antireflective coating：Using sial target mid frequency sputtering plated film mode, implement reactive sputtering plated film, first pass through
Argon gas distribution pipe is passed through argon to vacuum interior, connects intermediate frequency power supply then to sial target, after the normal sputtering of sial target, leads at once
Cross oxygen gas distribution pipe and be passed through oxygen to vacuum interior, carry out reactive sputtering, target molecule and gas molecule chemical combination are deposited on metal
Pipe surface, forms thin film, until described film layer reaches required design thickness；Its coating process parameter is：It is passed through vacuum coating
The argon flow amount of room is 120sccm, and oxygen flow is 60sccm, and intermediate frequency power supply frequency is 60KHZ, and technique vacuum is 3.5*
10-1Pa, sial target voltage is 550V, and the plated film time is 20 minutes.
The high temperature solar energy selective absorption coating being obtained on the surface of stainless steel tube matrix using said method, its structure
As shown in figure 1, including successively from the inside to the outside on the surface of stainless steel tube matrix：Metallic reflection film layer, diffusion barrier film layer, absorption
Film layer and antireflective coating；Wherein, described absorbing membranous layer includes four absorption subgrades that tenor reduces from the inside to the outside in gradient,
The tenor of four absorption subgrades changes in gradient so as to the diffusing phenomenon in hot operation are very slight, improves film layer
Stability in high temperature.Described absorbing membranous layer is nickel oxide aluminum absorbing membranous layer, and nickel aluminium element is introduced metallic reflection film layer, and
Sputtered by vacuum response, be allowed to generate the NiAlN selective absorption film with good absorption ability.Using excellent the resisting of Ni
Oxidation susceptibility is so as to as the metal component in metal medium, improve the resistance to elevated temperatures of film layer.Described antireflective coating is
SiO2-Al2O3Anti-reflection film, in outermost SiO2A small amount of aluminum is introduced, by the magnetic control reaction of Si-Al alloys target in antireflective coating
Sputtering, generates SiO2-Al2O3Double antireflection film layers, further increase the absorbent properties of film layer, strengthen membrane system of the present invention simultaneously
The hardness on surface and wearability.
In the present embodiment, the thickness of described metallic reflection film layer is 100nm, and the thickness of described diffusion barrier film layer is
25nm, in described absorbing membranous layer, the thickness of four absorption subgrades from the inside to the outside is respectively 40nm, 35nm, 30nm, 25nm, described
The thickness of antireflective coating is 100nm.
The preparation method of high temperature solar energy selective absorption coating provided in an embodiment of the present invention has the advantages that：
（1）Excellent combination property using the film layer membrane system of the high temperature solar energy selective absorption coating of this method preparation：Protecting
While holding high film performance, its resistance to elevated temperatures is splendid, and its absorbance reaches 96%, emissivity ＜ 6%；Its SiO2-Al2O3
Antireflection film layer, while possessing anti-reflective effect, film layer is anti-corrosion, anti-wear performance is lifted further, in air with very
Empty degradation shows, the decay of film performance in the high-temperature circulation test of 5000 hours is less than 1%.
（2）During film forming, speed is fast, and target is simple and easy to get, and utilization rate is high, is particularly suitable for factorial praluction.Inhale in plating selectivity
During winder layer, nickel aluminum target can generate the NiAlN film layer of high durable, high-absorbility.Using Ni-Al binary target system, its absorbance, one-tenth
Film speed and weather resistance are preferably mated.
（3）Using mid frequency sputtering and pulse direct current sputtering, compared with radio-frequency (RF) sputtering equipment simply it is easy to manipulate, film layer preparation
Technology stability is strengthened, and film performance is further improved.Especially medium frequency reactive sputtering is coated with SiO2-Al2O3Antireflective coating
Layer, using magnetron sputtering cylindrical target（Si-Al alloys target）, it is prevented effectively from the easy starting the arc of flat target and the problem that heat conduction is uneven,
Target utilization also greatly improves compared with flat target simultaneously.
（4）Cost reduction aspect：One is to replace expensive tungsten target with nickel alumin(i)um alloy target；Two is to be replaced with silico-aluminum cylindrical target
Silicon flat target, the target utilization of cylindrical target is almost 2 times of flat target target utilization, greatly reduces film from these two aspects
The preparation cost of layer.
Certainly, described above is also not limited to the example above, the present invention without description technical characteristic can by or
Realized using prior art, will not be described here；Above example and accompanying drawing are merely to illustrate technical scheme not
It is limitation of the present invention, reference has preferred embodiment been described in detail to the present invention, the ordinary skill people of this area
Member it should be appreciated that those skilled in the art made in the essential scope of the present invention change, remodeling, interpolation
Or replace without departure from spirit of the invention, also should belong to the claims of the present invention.
Claims (6)
1. a kind of high temperature solar energy selective absorption coating, with metal material as base material it is characterised in that table in metal base
Face, includes from the inside to the outside successively：Metallic reflection film layer, diffusion barrier film layer, absorbing membranous layer and antireflective coating；Wherein, described suction
Winder layer includes four absorption subgrades that tenor reduces from the inside to the outside in gradient.
2. high temperature solar energy selective absorption coating according to claim 1 is it is characterised in that described absorbing membranous layer is nitrogen
Change nickel aluminum absorbing membranous layer.
3. high temperature solar energy selective absorption coating according to claim 2 is it is characterised in that described antireflective coating is
SiO2-Al2O3Double anti-reflection films.
4. the high temperature solar energy selective absorption coating according to any one of claim 1-3 is it is characterised in that described metal
The thickness of reflective coating is 80-100nm, and the thickness of described diffusion barrier film layer is 15-25nm, in described absorbing membranous layer by interior extremely
The thickness of four outer absorption subgrades is respectively 35-40nm, 30-35nm, 25-30nm, 20-25nm, the thickness of described antireflective coating
Spend for 80-100nm.
5. a kind of preparation method of high temperature solar energy selective absorption coating, for preparing described in any one of claim 1-4
High temperature solar energy selective absorption coating is it is characterised in that methods described is applied to intermediate frequency and pulse direct current vacuum magnetic-control sputtering
Filming equipment, methods described is carried out in accordance with the following steps：
S101：Substrate pretreatment：Metal base is polished rear deionized water rinse, then dries passivation, make Metal Substrate
The surface of material forms passivation layer；
S102：Preheating：The metal base processing in step S101 is placed in the vacuum interior of coater, makes described metal base
Then the indoor temperature of vacuum can be increased to 350-400 DEG C, be incubated 30- around the central rotation of vacuum chamber while rotation
60min；
S103：Being coated with of metallic reflection film layer：Nickel aluminum target is sputtered using direct current pulse power source, is coated with metal in metallic substrate surface
Reflective coating, until described film layer reaches required design thickness, coating process parameter is：Background vacuum is in 4.0*10-3Pa
Hereinafter, in the range of 160-200sccm, process pressure is 2.0*10 to the argon flow amount being passed through vacuum film coating chamber-1-2.5*10- 1Pa；In the range of 400-450V, in the range of 40-45A, the plated film time is 8- to electric current to the sputtering voltage of direct current pulse power source
10min；
S104：Being coated with of diffusion barrier film layer：Using twin aluminum target medium frequency reactive sputtering mode, implement reactive sputtering plated film, directly
Reach required design thickness to described film layer；Its coating process parameter is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, in the range of 55-65sccm, its process pressure is 3.0*10 to the flow of reacting gas nitrogen-1-3.5*10-1Pa；In the range of 420-440V, in the range of frequency 40-60KHZ, electric current is 40-45A to intermediate frequency power supply sputtering voltage, the plated film time
For 1-3min；
S105：Being coated with of absorbing membranous layer：
S1051：The preparation of the first absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 70-80sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, aluminum target voltage in the range of 400-420V, electric current
In the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, in the range of 500-550V, electric current exists nickel aluminum target voltage
In the range of 40-45A, the plated film time is 3-5 minute；
S1052：The preparation of the second absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 60-70sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, wherein aluminum target voltage in the range of 400-420V,
Electric current is in the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is in the range of 450-500V, electric
In the range of 35-40A, the plated film time is 4-6 minute to stream；
S1053：The preparation of the 3rd absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 50-60sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, aluminum target voltage in the range of 400-420V, electric current
In the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, in the range of 400-450V, electric current exists nickel aluminum target voltage
In the range of 30-35A, the plated film time is 5-7 minute；
S1054：The preparation of the 4th absorption subgrade：Reactive sputtering plated film is carried out using nickel aluminum target and twin aluminum target simultaneously, until institute
State film layer and reach required design thickness；The technological parameter of its plated film is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, nitrogen flow is in the range of 40-50sccm；Technique vacuum is in 3.0*10-1-3.5*10-1In the range of Pa,
Powered to twin aluminum target using intermediate frequency power supply, frequency in the range of 40-60KHZ, wherein aluminum target voltage in the range of 400-420V,
Electric current is in the range of 40-45A；Powered to nickel aluminum target using direct current pulse power source, nickel aluminum target voltage is in the range of 350-400V, electric
In the range of 25-30A, the plated film time is 6-8 minute to stream；
S106：Being coated with of antireflective coating：Using sial target mid frequency sputtering plated film mode, implement reactive sputtering plated film, until described
Film layer reaches required design thickness；Its coating process parameter is：The argon flow amount being passed through vacuum film coating chamber is in 100-
In the range of 120sccm, oxygen flow in the range of 50-60sccm, intermediate frequency power supply frequency in the range of 40-60KHZ, technique vacuum
Spend for 3.0*10-1-3.5*10-1Pa, in the range of 500-550V, the plated film time is 15-20min to sial target voltage.
6. the preparation method of high temperature solar energy selective absorption coating according to claim 5 is it is characterised in that described aluminum
Target, nickel aluminum target and sial target are column magnetic control sputtering target, and the distance between aluminum target, sial target and metal base are 15-
The distance between 25cm, nickel aluminum target and metal base are 5-15cm.
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| JP2020173333A (en) * | 2019-04-10 | 2020-10-22 | デクセリアルズ株式会社 | Thin film for optical element and manufacturing method thereof, inorganic polarizer and manufacturing method thereof, and optical element and optical apparatus |
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| CN112795884A (en) * | 2021-04-08 | 2021-05-14 | 中南大学湘雅医院 | Preparation method of high-light-transmittance antifogging coating and laparoscope |
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Application publication date: 20170215 |