CN102121757A - Non-vacuum solar spectrum selective absorption coating and preparation method thereof - Google Patents
Non-vacuum solar spectrum selective absorption coating and preparation method thereof Download PDFInfo
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- 238000001228 spectrum Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 238000010521 absorption reaction Methods 0.000 title abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 74
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 claims abstract description 55
- 239000002184 metal Substances 0.000 claims abstract description 55
- 150000004767 nitrides Chemical class 0.000 claims abstract description 39
- 229910052786 argon Inorganic materials 0.000 claims abstract description 35
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- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000006096 absorbing agent Substances 0.000 claims description 34
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- 229910010037 TiAlN Inorganic materials 0.000 claims description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
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- 229910017083 AlN Inorganic materials 0.000 abstract description 25
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 12
- 229910045601 alloy Inorganic materials 0.000 abstract description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 30
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- 230000008021 deposition Effects 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
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- 229910017052 cobalt Inorganic materials 0.000 description 1
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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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- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a non-vacuum solar spectrum selective absorption coating and a preparation method thereof. The preparation method comprises the following steps: (1) selecting copper or stainless steel with low infrared emissivity as a base material; (2) selecting oxide resistant to high-temperature oxidation, nitride and complex or doped oxide as a film material, wherein a metal or an alloy serves as a bonding force increased layer, metal nitride or pure metal serves as a high infrared reflecting layer, an absorption layer is composed of two conducting particle ceramic layers with different metal nitride conducting particle volume fractions, and aluminium nitride and aluminium oxide serve as an antireflection layer; (3) controlling the components and contents of different film materials by controlling gas flow and sputtering power; (4) cleaning the base material before the base material is placed into a vacuum chamber, and carrying out argon ion bombarding on the surface of the base material before sputtering is carried out; and (5) obtaining a multilayer coating, wherein the thickness of the coating is less than 500nm, and the coating has high absorption rate alpha (0.9-0.97) in the solar spectrum range (0.3-2.5microns) and has extremely low emissivity epsilon (0.02-0.18) in the infrared region (2.5-50microns).
Description
Technical field
The invention belongs to solar thermal utilization material technology field, specially refer to the middle high temperature coating for selective absorption of sunlight spectrum that utilizes the technique of magnetron reactive sputtering preparation.This coating has spectral selection absorption characteristic preferably, and the serviceability temperature of this coating in antivacuum is higher than 400 degrees centigrade, and serviceability temperature in a vacuum is higher than 500 degrees centigrade.This coating can be used for antivacuum flat plate collector and trough type solar power generation is used in the high temperature heat collector.
Background technology
The characteristics of solar selectively absorbing coating are to have higher absorptivity α at solar energy spectral limit (0.3～2.5 micron), at region of ultra-red (2.5～50 microns) very low emissivity are arranged.The heat energy that it can convert the solar energy of low energy densities to high-energy-density gets up the solar energy enrichment, improves the solar energy thermal conversion efficiency, is a content that comes into one's own in the solar thermal utilization research work.
Different with coating structure according to the principle that absorbs sunshine, the fundamental type of coating for selective absorption has coated semiconductor, interference of light coating, multilayer gradual change coating, metal-cermic coating and porous coating.Wherein cermet composite coating has good heat endurance, and high temperature field in being mainly used in is one of coating newly developed in recent years.Cermet is metallic to be mixed in the dielectric matrixs such as oxide or nitride, and band-to-band transition and short grained resonance by metal make coating to solar spectrum very strong absorption be arranged.Metallic commonly used has copper, gold, nickel, molybdenum, chromium, platinum, cobalt or tungsten, they have desirable extinction coefficient in the visible region, dielectric matrix has silica, alundum (Al, magnesia, aluminium nitride and titanium nitride etc., in visible region refractive index n＜2, is the ideal medium matrix; The common metal ceramic coating has: chromium-chrome green, nickel-alundum (Al, molybdenum-alundum (Al, cobalt-alundum (Al; Yet when being higher than 350 degrees centigrade, these coatings can only be used for vacuum environment.The domestic report that yet there are no of high temperature resistant (being higher than 400 degrees centigrade) solar selectively absorbing coating for antivacuum use.
The coating for selective absorption that U.S. Pat 339.484 relates to is that depositing the stainless steel monocarbide then is absorbed layer at the copper film of the infrared high reflection of first sputtering sedimentation one deck on glass, and this coating solar absorptance (AM2) is 0.92, and emissivity is 0.05.
That Chinese invention patent CN 1056159A relates to is a kind of AlN
xO
xCoating for selective absorption is made negative electrode with single aluminium during preparation, uses argon gas, nitrogen, three kinds of gases of oxygen, and this coating solar absorptance is 0.90～0.94, infrared emittance is 0.07～0.12.
What Chinese invention patent CN85100142.4 related to is a kind of aluminium one nitrogen (or aluminium one carbon one oxygen) coating for selective absorption, and with single aluminium negative electrode, active gases is high pure nitrogen (carbon monoxide), and solar absorptance is 0.93, and emissivity is 0.06.
Chinese invention patent CN1360084A relates to is that a kind of absorbed layer is to be the negative electrode aluminium nitrogen that sputter forms in nitrogen, air, (nitrogen+oxygen) atmosphere+titanium nitrogen-aluminium titanium film and aluminum-nitrogen-oxygen+titanium-nitrogen-oxygen-aluminium titanium film with titanium and alloy aluminum, its antireflection layer is aluminium nitrogen+titanium nitrogen film and aluminum-nitrogen-oxygen+titanium-nitrogen-oxygen film, under atmospheric condition through 350 ℃, 250 hours, or 400 ℃, 50 hours, or 450 ℃, after the baking in 80 hours, its solar absorptance all can reach more than 0.93, and emissivity is 0.06～0.10.
Summary of the invention
The object of the present invention is to provide a kind of coating for selective absorption of sunlight spectrum and preparation method thereof with high serviceability temperature,, not sludge proof defective low with the serviceability temperature that overcomes existing coating, thereby satisfy the needs that elevated temperature heat utilizes the material field to develop in the solar energy, and its manufacturing process is simple, easily grasps.
To achieve these goals, the present invention takes following technical scheme:
A kind of non-vacuum solar spectrum selective absorber coatings, this absorber coatings is to be provided with transition zone, high infrared reflection layer, absorbed layer and antireflection layer in the substrate of stainless steel or copper from inside to outside successively, wherein, absorbed layer is divided into two-layer: first absorbed layer and second absorbed layer, and be arranged in order from inside to outside; Transition zone is the compound (atomic ratio of Ti and Al is 1/1～1/3) that magnesium-yttrium-transition metal Ti and metal A l form; The high infrared reflection layer is a kind of among metal nitride TiN, TiAlN, simple metal Al and the simple metal Cu; First absorbed layer in the absorbed layer and second absorbed layer are any one and AlN or the Al among metal nitride TiN, the TiAlN
2O
3The mixture that forms, wherein, in first absorbed layer, the volume fraction of any one among metal nitride TiN, the TiAlN is 40～80%, AlN or Al
2O
3Volume fraction be 20～60%; In second absorbed layer, the volume fraction of any one among metal nitride TiN, the TiAlN is 15～50%, AlN or Al
2O
3Volume fraction be 50～85%; Antireflection layer is AlN or Al
2O
3
In non-vacuum solar spectrum selective absorber coatings of the present invention, described transition region thickness is 40～200 nanometers, the high infrared reflection layer thickness is 50～300 nanometers, the 1st absorber thickness of absorbed layer is 30～200nm, the 2nd absorber thickness is 30～200nm, and antireflection layer thickness is 30～200 nanometers.
The present invention proposes metal nitride (TiN, TiAlN) is substituted the metallic that uses at present as conducting particles, adopts metal nitride or metal oxide as ceramic layer and antireflection layer (AlN, Al
2O
3) prepare conducting particles Ceramic Composite absorber coatings, the reasons are as follows: 1. relatively and metal, nitride and good high-temperature stability and high-temperature oxidation resistance are arranged.2. can obtain to have the metal nitride of low resistivity by the adjusting of metal volume mark, have low radiance at mid and far infrared; 3. AlN and Al
2O
3Various electrical properties (dielectric constant, dielectric loss, body resistivity, dielectric strength) good, light-transfer characteristic is good, good insulation preformance, the resistivity height, stable chemical performance, AlN wherein is ability and air generation oxidation when being higher than 1000 ℃, can be stabilized to 1500 ℃ in a vacuum.
The present invention utilizes a kind of that the interaction mechanism of electromagnetic wave and material designs to have higher absorptivity α at solar energy spectral limit (0.3～2.5 micron), at region of ultra-red (2.5～50 microns) very low emissivity is arranged; This structural design mainly considered electromagnetic wave and material interact in electromagnetic mutual interference stack, material to absorption of electromagnetic wave and reflection, material thickness to electromagnetic wave and the interactional influence of material.The structure of coating is: substrate/transition zone/high infrared reflection layer/metal nitride conducting particles pottery absorbed layer/antireflection layer.
Base material among the present invention is chosen is a kind of in stainless steel (304 or 316), Cu, Al, glass and the polishing Si sheet of surface finish.
Transition zone among the present invention mainly is in order to improve the adhesion of rete and base material, and this layer has high infrared reflectivity simultaneously, is mainly concerned with the compound that magnesium-yttrium-transition metal Ti and metal A l form, and corresponding transition zone is TiAl.The target that this layer adopted is Ti and Al simple metal target, or the TiAl alloys target.Reacting gas and working gas are high-purity Ar, adopt the preparation method of direct current or rf magnetron sputtering or direct current-radio frequency, DC-to-dc cosputtering.
High infrared reflection layer among the present invention mainly is metal nitride or the simple metal Al or the Cu of high tenor, the master metal of the metal nitride that relates to will comprise magnesium-yttrium-transition metal Ti, metal nitride is the metal nitride that magnesium-yttrium-transition metal Ti forms, or the metal nitride of magnesium-yttrium-transition metal Ti and metal A l formation, the corresponding metal nitride is TiN, TiAlN etc.The target that this layer adopted is Ti, Al or Cu simple metal target, or the TiAl alloys target.Reacting gas and working gas are high-purity N
2And high-purity Ar, perhaps reacting gas and working gas are high-purity Ar.Adopt the preparation method of direct current or rf magnetron sputtering or direct current-radio frequency, DC-to-dc cosputtering.
Absorbed layer among the present invention is made up of the conducting particles pottery absorbed layer of two-layer different metal nitride conducting particles volume fraction, the master metal of the metal nitride conducting particles that relates to will comprise magnesium-yttrium-transition metal Ti, and this metal nitride is a kind of and AlN or the Al among metal nitride TiN, the TiAlN of magnesium-yttrium-transition metal M
2O
3The mixture that forms.The target that this layer adopted is Ti and Al simple metal target, or with Ti and Al simple metal target as target, perhaps adopt Al and TiAl alloys target as target.Reacting gas and working gas are high-purity Ar and high-purity N
2, perhaps high-purity Ar, high-purity N
2With high-purity O
2Adopt the preparation method of direct current-radio frequency or DC-to-dc cosputtering.
Antireflection layer among the present invention mainly is in order to reduce visible-near infrared reflection loss, to improve the absorptivity of coating, mainly is nitride and the oxide of Al, comprises AlN or Al
2O
3The target that this layer adopted is an Al simple metal target.Reacting gas and working gas are high-purity Ar and high-purity N
2, or high-purity Ar and high-purity O
2, the preparation method of employing direct current or rf magnetron sputtering.
The present invention is directed to different film materials and control each thicknesses of layers and composition by flow and the sedimentation time of adjusting sputtering power, nitrogen and argon and oxygen.
High temperature coating for selective absorption of sunlight spectrum and preparation method thereof during the present invention is a kind of, its solution of key technology scheme is:
(1) adopts stainless steel or copper as base material, and base material is cleaned;
(2) after the base material after will cleaning is inserted the vacuum sputtering chamber of many targets composite film coating machine, toast;
(3) after the baking, be 0.35 handkerchief～1.5 handkerchiefs to the indoor feeding argon gas of vacuum sputtering to air pressure, and adopt 500 volts～900 volts back bias voltage that substrate material surface is carried out argon ion bombardment;
(4) at sputter pressure 0.1 handkerchief～1 handkerchief, under bombarding voltage 20 volts～120 laid shoot spares, carry out plated film, wherein:
As target, adopt direct current-radio frequency cosputtering or DC-to-dc cosputtering to prepare transition zone with Al and Ti, perhaps with TiAl as target, adopt direct current or rf magnetron sputtering to prepare transition zone; Reacting gas and working gas are high-purity Ar; The deposition transition zone to be increasing membranous layer binding force, recently obtains low infrared emittance and adhesion preferably by the atom of regulating aluminium in the transition zone;
As target, reacting gas and working gas are high-purity Ar and high-purity N with Ti or TiAl
2Perhaps adopt Al or Cu as target, reacting gas and working gas are high-purity Ar; Adopt magnetically controlled DC sputtering, rf magnetron sputtering, direct current-radio frequency cosputtering or DC-to-dc cosputtering to prepare the high infrared reflection layer, obtain low infrared emittance by the volume fraction of regulating metal in the rete;
Adopt the method for direct current-radio frequency or DC-to-dc cosputtering to prepare absorbed layer, adopt Al and Ti, perhaps adopt Al and TiAl as target as target; Reacting gas and working gas are high-purity Ar and high-purity N
2, perhaps high-purity Ar, high-purity N
2With high-purity O
2Plated metal nitride conducting particles pottery absorbed layer, rete is made of two-layer, and the volume fraction of metal nitride is 40～80% in the ground floor, and the volume fraction of metal nitride is 15～50% in the second layer;
Adopt the preparation antireflection layer of direct current or rf magnetron sputtering, adopt Al as target, reacting gas and working gas are high-purity Ar and high-purity N
2, perhaps high-purity Ar and high-purity O
2, last depositing nitride or oxide antireflection layer.
For the integrality that guarantees the growth of every tunic and prevent atom diffusion between each layer, plate every layer between 5～15min at interval, cool off at last and take out sample after causing room temperature.
In the method for preparing the non-vacuum solar spectrum selective absorber coatings of the present invention,, be that base material was toasted 10～30 minutes under 100～150 ℃ of conditions described step (2) base material is carried out in the bake process.
In the method for preparing the non-vacuum solar spectrum selective absorber coatings of the present invention, described step (1) base material is carried out in the cleaning process, be that base material is ultrasonic in sulfuric acid, washing agent, deionized water, gasoline and ethanol respectively, in every kind of liquid ultrasonic 1～6 minute, 5～30 minutes altogether.
In the method for preparing the non-vacuum solar spectrum selective absorber coatings of the present invention,, argon ion bombardment was carried out 30～60 minutes in its surface described step (3) substrate material surface is carried out in the argon ion bombardment process.
In the method for preparing the non-vacuum solar spectrum selective absorber coatings of the present invention, in the coating process of described step (4), by adjusting sputtering power, high-purity Ar, high-purity N
2With high-purity O
2In one or more flow and sedimentation time control each thicknesses of layers and composition.
Principle of the present invention is: adopt vacuum magnetic-control sputtering coating technique plated metal nitride on the surface of metal or alloy and conductive metal nitride is compound or doping insulative nitride (or oxide) film, solved the coating high-temp problem of oxidation on the one hand, the metallicity gloss and the color of material have been changed on the other hand, obtained to have higher absorptivity α, the coating material of very low emissivity has been arranged at region of ultra-red (2.5～50 microns) at solar energy spectral limit (0.3～2.5 micron).
A kind of non-vacuum solar spectrum selective absorber coatings of the present invention and preparation method thereof, its advantage is: coating has higher absorptivity α in solar spectrum scope (0.3～2.5 micron), at region of ultra-red (2～50 microns) very low emissivity is arranged, have the high temperature oxidation resisting characteristic simultaneously, satisfy the requirement that solar energy high temperature utilizes.This preparation method is simple, and cost is low, and the coating that adopts this method to make can be used for groove type solar generating and building body heat collector, and the weight of coating is lighter.
Description of drawings
Fig. 1 is the microstructure models of coating of the present invention, wherein 1 is substrate, 2 for increasing adhesion transition zone (this layer also is the low infrared emissivity layer), 3 is high metal volume mark nitride high infrared reflection layer, 4 is i.e. the 1st absorbed layer of absorbed layer of high conducting particles amount of nitrides, 5 absorbed layers for low conducting particles amount of nitrides are the 2nd absorbed layer, and 6 is antireflection layer.
Fig. 2 is the surface topography that utilizes the multilayer film sample that the present invention obtains.
Fig. 3 is the cross-section morphology that utilizes the multilayer film sample that the present invention obtains.
Fig. 4 utilizes preparation aspect product that the present invention obtains and the XRD figure spectrum of 400 and 500 degrees centigrade of annealing in process sample after 2 hours in atmosphere.
Fig. 5 utilizes preparation aspect product that the present invention obtains and the reflectivity collection of illustrative plates at 0.3～2.5 micron waveband of 400 and 500 degrees centigrade of annealing in process sample after 2 hours in atmosphere.
Fig. 6 for the present invention the coating that is coated with at stainless steel-based the end in air 350～800 degrees centigrade after handling 2 hours absorptivity and the variation tendency of emissivity.
Fig. 7 for the present invention with Cu as the high infrared reflection layer, the visible near-infrared reflection spectrogram of the coating that is coated with at stainless steel-based the end.
The specific embodiment
A kind of non-vacuum solar spectrum selective absorber coatings of the present invention and preparation method thereof is a kind of sandwich construction coating with spectral selection absorption of designing according to the interaction mechanism of electromagnetic wave and film, as shown in Figure 1.
Below in conjunction with specific embodiment, technical scheme of the present invention is further specified.Wherein, the percentage of being annotated in the metal nitride back bracket of first absorbed layer of the absorbed layer in the film material among each embodiment and second absorbed layer is percentage by volume.
(1) chooses stainless steel as substrate 1;
(2) choose titanium aluminium as film material (transition zone) 2;
(3) choose titanium nitride as film material (high infrared reflection layer) 3;
(4) (titanium nitride-aluminium nitride) film of choosing high titanium nitride content is a film material (the 1st absorbed layer) 4;
(5) choosing (titanium nitride-aluminium nitride) film that hangs down titanium nitride content is film material (the 2nd absorbed layer) 5;
(6) choose aluminium nitride as film material (antireflection layer) 6;
(7) adopt many targets composite film coating machine to carry out plated film; In order to improve the adhesion of film and substrate, inserted before the vacuum chamber backing material in sulfuric acid, washing agent, deionized water, gasoline, ethanol ultrasonic 5～30 minutes respectively, oven dry; After inserting vacuum chamber, 100～150 degrees centigrade were toasted 10～30 minutes, and the experiment base vacuum is 1 * 10
-3Handkerchief, before the sample deposition, feeding argon gas to air pressure is 0.35～1.5 handkerchief, 500～900 volts back bias voltage is carried out argon ion bombardment to sample surfaces, to remove the gas and the impurity of surface absorption, exposes clean surface.Base vacuum is better than 1 * 10 in the vacuum sputtering chamber
-3Introduce an amount of reacting gas argon gas during handkerchief as required, perhaps nitrogen and argon gas.In order to obtain uniform rete, to treat after the stable gas pressure substrate low speed to be clockwise rotated, deposit film, target-substrate distance are 5～25 centimetres, other technological parameter of experiment sees the following form:
(8) finally obtained having the coating of multilayer grading structure, the thickness of this coating is 487 nanometers, (wherein transition region thickness is 62.9 nanometers, the high infrared reflection layer thickness is 108 nanometers, the 1st absorber thickness of absorbed layer is 117nm, and the 2nd absorber thickness is 128nm, and antireflection layer thickness is 65 nanometers), have high absorptivity α (～0.94) at solar energy spectral limit (0.3～2.5 micron), very low emissivity (～0.08) is arranged at region of ultra-red (2～50 microns).
The surface topography that utilizes the stainless steel-based priming coat that the present invention obtains as shown in Figure 2.As can be seen, open defect does not appear in the film sample surface, and TiN is evengranular to be distributed among the AlN matrix, and the average diameter of particle is 30 nanometers.
The cross-section morphology of the stainless steel-based priming coat that the present invention obtains as shown in Figure 3.As can be seen, the rete densification, germination is intact.
400 and 500 degrees centigrade of X-ray diffraction spectrograms after handling 2 hours are as shown in Figure 4 at stainless steel-based the end in the coating that is coated with and in air in the present invention.As can be seen coating through in air 400 and 500 degrees centigrade handle that structure does not change after 2 hours.
400 and 500 degrees centigrade of visible near-infrared reflection spectrograms after handling 2 hours are as shown in Figure 5 at stainless steel-based the end in the coating that is coated with and in air in the present invention.As can be seen coating through in air 400 and 500 degrees centigrade handle that spectral reflectivity does not change after 2 hours.
The present invention the coating that is coated with at stainless steel-based the end in air 350～800 degrees centigrade after handling 2 hours absorptivity and the variation tendency of emissivity as shown in Figure 6.Spectral reflectivity does not change coating after 2 hours through handling below 500 degrees centigrade in air as can be seen.
By Fig. 3～6 anti-500 celsius temperature oxidations of coating as can be known.
As the high infrared reflection layer, as seen the visible near-infrared reflection spectrogram of the coating that is coated with should the series coating have good spectral selection absorption characteristic as shown in Figure 7 at stainless steel-based the end with Cu in the present invention.
Embodiment 2
(1) chooses stainless steel as substrate 1;
(2) choose titanium aluminium film as transition zone 2;
(3) choose titanium aluminum nitride film as high infrared reflection layer 3;
(4) (TiAlN-aluminium nitride) film of choosing high TiAlN content is as film material, i.e. the 1st absorbed layer 4;
(5) (TiAlN-aluminium nitride) film of choosing low TiAlN content is as film material, i.e. the 2nd absorbed layer 5;
(6) choose aluminium nitride film as antireflection layer 6.
(7) adopt many targets composite film coating machine to carry out plated film; In order to improve the adhesion of film and substrate, inserted before the vacuum chamber backing material in sulfuric acid, washing agent, deionized water, gasoline, ethanol ultrasonic 5～30 minutes respectively, oven dry; After inserting vacuum chamber, 100～150 degrees centigrade were toasted 10～30 minutes, and the experiment base vacuum is 1 * 10
-3Handkerchief, before the sample deposition, feeding argon gas to air pressure is 0.35～1.5 handkerchief, 500～900 volts back bias voltage is carried out argon ion bombardment to sample surfaces, to remove the gas and the impurity of surface absorption, exposes clean surface.Base vacuum is better than 1 * 10 in the vacuum sputtering chamber
-3Introduce an amount of reacting gas argon gas during handkerchief as required, perhaps nitrogen and argon gas.In order to obtain uniform rete, to treat after the stable gas pressure substrate low speed to be clockwise rotated, deposit film, target-substrate distance are 5～25 centimetres, other technological parameter of experiment sees the following form:
(8) finally obtained having the coating of multilayer grading structure, the thickness of this coating is 478 nanometers, (wherein transition region thickness is 62.9 nanometers, the high infrared reflection layer thickness is 108 nanometers, the 1st absorber thickness of absorbed layer is 108nm, and the 2nd absorber thickness is 137nm, and antireflection layer thickness is 62.9 nanometers), have high absorptivity α (0.9～0.95) at solar energy spectral limit (0.3～2.5 micron), very low emissivity (0.08～0.18) is arranged at region of ultra-red (2～50 microns).
Embodiment 3
(1) chooses stainless steel as substrate 1;
(2) choose titanium aluminium film as transition zone 2;
(3) choose titanium nitride membrane as high infrared reflection layer 3;
(4) choose (titanium nitride-alundum (Al) film of high titanium nitride content as being film material, i.e. the 1st absorbed layer 4;
(5) (titanium nitride-alundum (Al) film of choosing low titanium nitride content is as film material, i.e. the 2nd absorbed layer 5;
(6) choose the alundum (Al film as antireflection layer 6.
(7) adopt many targets composite film coating machine to carry out plated film; In order to improve the adhesion of film and substrate, inserted before the vacuum chamber backing material in sulfuric acid, washing agent, deionized water, gasoline, ethanol ultrasonic 5～30 minutes respectively, oven dry; After inserting vacuum chamber, 100～150 degrees centigrade were toasted 10～30 minutes, and the experiment base vacuum is 1 * 10
-3Handkerchief, before the sample deposition, feeding argon gas to air pressure is 0.35～1.5 handkerchief, 500～900 volts back bias voltage is carried out argon ion bombardment to sample surfaces, to remove the gas and the impurity of surface absorption, exposes clean surface.Base vacuum is better than 1 * 10 in the vacuum sputtering chamber
-3Introduce an amount of reacting gas argon gas during handkerchief as required, perhaps nitrogen and argon gas, perhaps nitrogen, argon gas and oxygen.In order to obtain uniform rete, to treat after the stable gas pressure substrate low speed to be clockwise rotated, deposit film, target-substrate distance are 5～25 centimetres, other technological parameter of experiment sees the following form:
(8) finally obtained having the coating of multilayer grading structure, the thickness of this coating is 290 nanometers, (wherein transition region thickness is 50 nanometers, the high infrared reflection layer thickness is 70 nanometers, the 1st absorber thickness of absorbed layer is 65nm, and the 2nd absorber thickness is 60nm, and antireflection layer thickness is 45 nanometers), have high absorptivity α (0.9～0.95) at solar energy spectral limit (0.3～2.5 micron), very low emissivity (0.08～0.18) is arranged at region of ultra-red (2～50 microns).
Embodiment 4
(1) chooses stainless steel as substrate 1;
(2) choose titanium aluminium film as transition zone 2;
(3) choose titanium aluminum nitride film as high infrared reflection layer 3;
(4) (TiAlN-alundum (Al) film of choosing high TiAlN content is as film material, i.e. the 1st absorbed layer 4;
(5) (TiAlN-alundum (Al) film of choosing low TiAlN content is as film material, i.e. the 2nd absorbed layer 5;
(6) choose the alundum (Al film as antireflection layer 6.
(7) adopt many targets composite film coating machine to carry out plated film; In order to improve the adhesion of film and substrate, inserted before the vacuum chamber backing material in sulfuric acid, washing agent, deionized water, gasoline, ethanol ultrasonic 5～30 minutes respectively, oven dry; After inserting vacuum chamber, 100～150 degrees centigrade were toasted 10～30 minutes, and the experiment base vacuum is 1 * 10
-3Handkerchief, before the sample deposition, feeding argon gas to air pressure is 0.35～1.5 handkerchief, 500～900 volts back bias voltage is carried out argon ion bombardment to sample surfaces, to remove the gas and the impurity of surface absorption, exposes clean surface.Base vacuum is better than 1 * 10 in the vacuum sputtering chamber
-3Introduce an amount of reacting gas argon gas during handkerchief as required, perhaps nitrogen and argon gas, perhaps nitrogen, argon gas and oxygen.In order to obtain uniform rete, to treat after the stable gas pressure substrate low speed to be clockwise rotated, deposit film, target-substrate distance are 5～25 centimetres, other technological parameter of experiment sees the following form:
(8) finally obtained having the coating of multilayer grading structure, the thickness of this coating is 455 nanometers, (wherein transition region thickness is 70 nanometers, the high infrared reflection layer thickness is 110 nanometers, the 1st absorber thickness of absorbed layer is 110nm, and the 2nd absorber thickness is 90nm, and antireflection layer thickness is 75 nanometers), have high absorptivity α (0.9～0.95) at solar energy spectral limit (0.3～2.5 micron), very low emissivity (0.08～0.18) is arranged at region of ultra-red (2～50 microns).
(1) chooses stainless steel as substrate 1;
(2) choose titanium aluminium film as transition zone 2;
(3) choose the Al film as high infrared reflection layer 3;
(4) choose (titanium nitride-aluminium nitride) film of high titanium nitride content as being film material, i.e. the 1st absorbed layer 4;
(5) (titanium nitride-aluminium nitride) film of choosing low titanium nitride content is as film material, i.e. the 2nd absorbed layer 5;
(6) choose aluminium nitride film as antireflection layer 6.
(7) adopt many targets composite film coating machine to carry out plated film; In order to improve the adhesion of film and substrate, inserted before the vacuum chamber backing material in sulfuric acid, washing agent, deionized water, gasoline, ethanol ultrasonic 5～30 minutes respectively, oven dry; After inserting vacuum chamber, 100～150 degrees centigrade were toasted 10～30 minutes, and the experiment base vacuum is 1 * 10
-3Handkerchief, before the sample deposition, feeding argon gas to air pressure is 0.35～1.5 handkerchief, 500～900 volts back bias voltage is carried out argon ion bombardment to sample surfaces, to remove the gas and the impurity of surface absorption, exposes clean surface.Base vacuum is better than 1 * 10 in the vacuum sputtering chamber
-3Introduce an amount of reacting gas argon gas during handkerchief as required, perhaps nitrogen and argon gas.In order to obtain uniform rete, to treat after the stable gas pressure substrate low speed to be clockwise rotated, deposit film, target-substrate distance are 5～25 centimetres, other technological parameter of experiment sees the following form:
(8) finally obtained having the coating of multilayer grading structure, the thickness of this coating is 290 nanometers, (wherein transition region thickness is 50 nanometers, the high infrared reflection layer thickness is 70 nanometers, the 1st absorber thickness of absorbed layer is 65nm, and the 2nd absorber thickness is 60nm, and antireflection layer thickness is 45 nanometers), have high absorptivity α (0.91～0.95) at solar energy spectral limit (0.3～2.5 micron), very low emissivity (0.06～0.13) is arranged at region of ultra-red (2～50 microns).
(1) chooses stainless steel as substrate 1;
(2) choose titanium aluminium film as transition zone 2;
(3) choose the Cu film as high infrared reflection layer 3;
(4) choose (titanium nitride-aluminium nitride) film of high titanium nitride content as being film material, i.e. the 1st absorbed layer 4;
(5) (titanium nitride-aluminium nitride) film of choosing low titanium nitride content is as film material, i.e. the 2nd absorbed layer 5;
(6) choose aluminium nitride film as antireflection layer 6.
(7) adopt many targets composite film coating machine to carry out plated film; In order to improve the adhesion of film and substrate, inserted before the vacuum chamber backing material in sulfuric acid, washing agent, deionized water, gasoline, ethanol ultrasonic 5～30 minutes respectively, oven dry; After inserting vacuum chamber, 100～150 degrees centigrade were toasted 10～30 minutes, and the experiment base vacuum is 1 * 10
-3Handkerchief, before the sample deposition, feeding argon gas to air pressure is 0.35～1.5 handkerchief, 500～900 volts back bias voltage is carried out argon ion bombardment to sample surfaces, to remove the gas and the impurity of surface absorption, exposes clean surface.Base vacuum is better than 1 * 10 in the vacuum sputtering chamber
-3Introduce an amount of reacting gas argon gas during handkerchief as required, perhaps nitrogen and argon gas.In order to obtain uniform rete, to treat after the stable gas pressure substrate low speed to be clockwise rotated, deposit film, target-substrate distance are 5～25 centimetres, other technological parameter of experiment sees the following form:
(8) finally obtained having the coating of multilayer grading structure, the thickness of this coating is 290 nanometers, (wherein transition region thickness is 50 nanometers, the high infrared reflection layer thickness is 70 nanometers, the 1st absorber thickness of absorbed layer is 65nm, and the 2nd absorber thickness is 60nm, and antireflection layer thickness is 45 nanometers), have high absorptivity α (0.92～0.97) at solar energy spectral limit (0.3～2.5 micron), very low emissivity (0.02～0.08) is arranged at region of ultra-red (2～50 microns).
Claims (6)
1. non-vacuum solar spectrum selective absorber coatings, it is characterized in that: this absorber coatings is to be provided with transition zone, high infrared reflection layer, absorbed layer and antireflection layer in the substrate of stainless steel or copper from inside to outside successively, wherein, absorbed layer is divided into two-layer: first absorbed layer and second absorbed layer, and be arranged in order from inside to outside; Transition zone is the compound that magnesium-yttrium-transition metal Ti and metal A l form, and wherein, the atomic ratio of Ti and Al is 1/1～1/3; The high infrared reflection layer is a kind of among metal nitride TiN, TiAlN, simple metal Al and the simple metal Cu; First absorbed layer in the absorbed layer and second absorbed layer are any one and AlN or the Al among metal nitride TiN, the TiAlN
2O
3The mixture that forms, wherein, in first absorbed layer, the volume fraction of any one among metal nitride TiN, the TiAlN is 40～80%, AlN or Al
2O
3Volume fraction be 20～60%; In second absorbed layer, the volume fraction of any one among metal nitride TiN, the TiAlN is 15～50%, AlN or Al
2O
3Volume fraction be 50～85%; Antireflection layer is AlN or Al
2O
3
2. non-vacuum solar spectrum selective absorber coatings according to claim 1, it is characterized in that: described transition region thickness is 40～200 nanometers, the high infrared reflection layer thickness is 50～300 nanometers, the 1st absorber thickness of absorbed layer is 30～200nm, the 2nd absorber thickness is 30～200nm, and antireflection layer thickness is 30～200 nanometers.
3. a method for preparing the described non-vacuum solar spectrum selective absorber coatings of claim 1 is characterized in that, this method comprises the steps:
(1) adopts stainless steel or copper as base material, and base material is cleaned;
(2) after the base material after will cleaning is inserted the vacuum sputtering chamber of many targets composite film coating machine, toast;
(3) after the baking, be 0.35 handkerchief～1.5 handkerchiefs to the indoor feeding argon gas of vacuum sputtering to air pressure, and adopt 500 volts～900 volts back bias voltage that substrate material surface is carried out argon ion bombardment;
(4) at sputter pressure 0.1 handkerchief～1 handkerchief, under bombarding voltage 20 volts～120 laid shoot spares, carry out plated film, wherein:
Adopt direct current or rf magnetron sputtering, or direct current-radio frequency or DC-to-dc cosputtering prepare transition zone; And adopt Al and Ti as target, perhaps with TiAl as target; Reacting gas and working gas are high-purity Ar;
Adopt magnetically controlled DC sputtering, rf magnetron sputtering, direct current-radio frequency cosputtering or DC-to-dc cosputtering to prepare the high infrared reflection layer, and adopt Ti or TiAl as target, reacting gas and working gas are high-purity Ar and high-purity N
2Perhaps adopt Al or Cu as target, reacting gas and working gas are high-purity Ar;
Adopt the method for direct current-radio frequency or DC-to-dc cosputtering to prepare absorbed layer, adopt Al and Ti, perhaps adopt Al and TiAl as target as target; Reacting gas and working gas are high-purity Ar and high-purity N
2, perhaps high-purity Ar, high-purity N
2The pure O of drawn game
2
Adopt the preparation antireflection layer of direct current or rf magnetron sputtering, adopt Al as target, reacting gas and working gas are high-purity Ar and high-purity N
2, perhaps high-purity Ar and high-purity O
2
4. the method for preparing the non-vacuum solar spectrum selective absorber coatings according to claim 2, it is characterized in that, described step (2) base material is carried out in the bake process, be that base material was toasted 10～30 minutes under 100～150 ℃ of conditions.
5. the method for preparing the non-vacuum solar spectrum selective absorber coatings according to claim 3, it is characterized in that, described step (1) base material is carried out in the cleaning process, be that base material is ultrasonic in sulfuric acid, washing agent, deionized water, gasoline and ethanol respectively, in every kind of liquid ultrasonic 1～6 minute, 5～30 minutes altogether.
6. the method for preparing the non-vacuum solar spectrum selective absorber coatings according to claim 3 is characterized in that, in the coating process of described step (4), by adjusting sputtering power, high-purity Ar, high-purity N
2With high-purity O
2In one or more flow and sedimentation time control each thicknesses of layers and composition.
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