CN107190239A - A kind of high temperature resistant solar selectively absorbing coating and preparation method thereof - Google Patents

A kind of high temperature resistant solar selectively absorbing coating and preparation method thereof Download PDF

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Publication number
CN107190239A
CN107190239A CN201710289087.2A CN201710289087A CN107190239A CN 107190239 A CN107190239 A CN 107190239A CN 201710289087 A CN201710289087 A CN 201710289087A CN 107190239 A CN107190239 A CN 107190239A
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coating
sputtering
preparation
rare
absorbed layer
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高祥虎
刘刚
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/0635—Carbides
    • 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
    • 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

Abstract

The invention discloses a kind of high temperature resistant solar selectively absorbing coating, the coating from bottom to top includes absorber substrate, absorbed layer and antireflection layer successively；Absorber substrate is polishing stainless steel piece, absorbs the compound that layer material is zirconium carbide and rare-earth yttrium, and antireflection layer material is aluminum oxide.The invention also discloses the preparation method of the coating.Coating prepared by the present invention is under the conditions of air quality factors A M1.5, and absorptivity is >=0.88, emissivity≤0.13；The coating has good high-temperature stability, can be used for a long time under 700 DEG C of vacuum environment.The present invention has wide practical value and application prospect in the field such as solar thermal utilization and heat generating, mink cell focus exploitation.

Description

A kind of high temperature resistant solar selectively absorbing coating and preparation method thereof
Technical field
The present invention relates to a kind of high temperature resistant solar selectively absorbing coating, belong to solar energy thermal-power-generating and vacuum coating skill Art field.
Background technology
Solar energy has two kinds of utilization ways：A kind of that solar radiation is converted into electric energy by photocell, common utilizes way Footpath is solar cell；Solar radiation is converted into heat energy by another by solar thermal collector, and simplest is exactly at home The roof water heater used.Generated electricity using solar thermal energy has turned into a major fields of global risk investment, its principle at present It is that pipeline or container equipped with certain liquid are gathered in sunray by beam condensing unit.By solar thermal energy, liquid is added Heat arrives certain temperature, produces steam and then drives turbine generation, heat energy is converted into electric energy.This generation mode is known as Solar energy thermal-power-generating.Recently, 20 solar energy thermal-power-generating demonstrative projects are built in National Energy Board's approval at home.The demonstrative project Construction, will greatly promote solar energy thermal-power-generating technology.Spectral selection solar energy absorbing coating is the core of solar energy thermal-power-generating Core material, it requires that the coating has high-absorbility, low-launch-rate and long-term thermal stability.
In recent years, cermet compound system solar energy absorbing coating has obtained extensive research, such as Al-AlN, Mo- SiO2、W-A12O3、Cr-Cr2O3、Ni-A12O3、Mo-A12O3、Cr-A12O3、Co-WC、W-Ni-A12O3、Ag-A12O3、Mo- Si3N4、Al-Ni-A12O3, W-Ni-YSZ etc..Wherein Mo-SiO2And Mo-A12O3System is by Italian Angelantoni- ENEA companies and Siemens companies of Germany successful commercialization are promoted.The coating has excellent optics at 580 DEG C of operating temperature Performance and good long-term thermal stability.For solar energy thermal-power-generating, opto-electronic conversion will be greatly improved in high operating temperature Efficiency, therefore, is developed in higher temperature（More than 600 DEG C）There is down superior heat-stability and the high temperature solar of optical property to inhale Receiving coating has important academic significance and practical value.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of high temperature resistant solar energy for shortcoming of the prior art Coating for selective absorption.
Coating absorptivity of the present invention is high, emissivity is low, heat endurance is good, exploited available for photo-thermal power generation, mink cell focus, The industrial or agricultural such as desalinization field.
It is a further object of the present invention to provide the preparation method of above-mentioned high temperature resistant solar selectively absorbing coating.
A kind of high temperature resistant solar selectively absorbing coating, the coating from bottom to top includes absorber substrate, absorbed successively Layer and antireflection layer；The absorber substrate is polishing stainless steel piece, and the described layer material that absorbs is zirconium carbide and rare-earth yttrium Compound, described antireflection layer material is aluminum oxide.
The thickness of the absorbed layer compound is 240-300 nm.
The atomic percent of the absorbed layer compound middle rare earth yttrium is 0.1-1%.
The thickness of the antireflection layer is 50-100 nm.
The polishing stainless steel piece roughness value of the absorber substrate is 0.5-2 nm.
The preparation method of above-mentioned high temperature resistant solar selectively absorbing coating, is comprised the following steps that：
1）The processing of absorber substrate：After the impurity that absorber substrate is removed to surface attachment, divide respectively in acetone and ethanol Chao Shengqingxi not be 10-20 minutes, nitrogen drying, vacuum is preserved；
2）The preparation of absorbed layer：The rare-earth yttrium that purity is 99.99% for 99.99% zirconium carbide and purity is used as magnetron sputtering Target；Absorbed layer is prepared using double target co-sputtering method, wherein zirconium carbide uses magnetically controlled DC sputtering, and rare-earth yttrium uses radio-frequency magnetic Sputtering method is controlled, vacuum chamber is taken out to base vacuum in advance to 1.0 × 10-6-5.0×10-6Torr；Adjust the sputtering of zirconium carbide target Power density is 4-8 W/cm-2, the Sputtering power density of rare-earth yttrium target is 0.08-0.3 W/cm-2, argon gas during sputtering sedimentation Air inflow be 20-50 sccm, start in absorber substrate depositing silicon zirconium and rare-earth yttrium compound, thickness is 240- 300 nm；
3）The preparation of antireflection layer：After absorbed layer preparation is finished, with the Al of purity 99.99%2O3It is used as magnetic control spattering target, control Al processed2O3The Sputtering power density of target is in 5-8 W/cm-2, the air inflow of argon gas is 20-50 sccm during sputtering sedimentation, is used Rf magnetron sputtering sputtering on absorbed layer prepares antireflection layer, and thickness is 50-100 nm；
The step 2）Absorber base reservoir temperature is 150-250 DEG C in middle absorbed layer sputter procedure.
The step 3）Absorber base reservoir temperature is 150-250 DEG C in middle antireflection layer sputter procedure.
Regulation and control of the invention based on the potential spectrum-selectivity characteristic of zirconium carbide and rare-earth yttrium, it is compound with zirconium carbide and rare-earth yttrium Thing is absorbed layer, and aluminum oxide is antireflection layer, greatly enriches zirconium carbide ceramics and rare-earth yttrium answering in solar energy industry With.The solar selective coat of the present invention has low reflectivity in UV, visible light near infrared spectral range, in infrared light There is high reflectivity, under the conditions of air quality factors A M1.5, absorptivity >=0.88, emissivity≤0.13 in spectral limit； Under condition of high vacuum degree, after 700 DEG C of long-time heat preservations, the absorptivity and emissivity of coating are not changed significantly, and show the coating With excellent high temperature stability performance.The present invention has wide practical value in solar thermal utilization and hot power field and should Use prospect.
Embodiment
A kind of high temperature resistant solar selectively absorbing coating of the invention and preparation method are made below by specific embodiment Further illustrate.
Embodiment 1
A kind of high temperature resistant solar selectively absorbing coating, includes absorber substrate, absorbed layer and subtracts successively from bottom to surface Reflecting layer；Absorber substrate is polishing stainless steel piece, and roughness value is 1.5nm, and it is zirconium carbide and rare-earth yttrium to absorb layer material Compound, the thickness of absorbed layer compound is 240nm.Absorbed layer compound is prepared using double target co-sputtering, and wherein zirconium carbide is adopted Prepared with DC magnetron sputtering method, rare-earth yttrium is prepared using radio frequency magnetron sputtering method；Absorbed layer compound middle rare earth yttrium is former Sub- percentage is 0.21%.Antireflection layer material is aluminum oxide, and the thickness of antireflection layer is 76 nm, and antireflection layer aluminum oxide is used Rf magnetron sputtering.
A kind of preparation method of above-mentioned high temperature resistant solar selectively absorbing coating, including following technique：
（1）The processing of absorber substrate：After the impurity that absorber substrate is removed to surface attachment, divide respectively in acetone and ethanol Chao Shengqingxi not be 10 minutes, nitrogen drying, vacuum is preserved；
（2）The preparation of absorbed layer：Purity is used to be splashed for the rare-earth yttrium that 99.99% zirconium carbide and purity is 99.99% as magnetic control Shoot at the target material；Absorbed layer is prepared using double target co-sputtering method, wherein zirconium carbide uses magnetically controlled DC sputtering, and rare-earth yttrium uses radio frequency Magnetically controlled sputter method, vacuum chamber is taken out in advance base vacuum to 3.0 × 10-6Torr；Adjust the Sputtering power density of zirconium carbide target For 6.5 W/cm-2, the Sputtering power density of rare-earth yttrium target is 0.1 W/cm-2, the air inflow of argon gas is 33 during sputtering sedimentation Sccm, starts the compound of depositing silicon zirconium and rare-earth yttrium in absorber substrate, and thickness is 240 nm.Absorbed heat in sputter procedure Body base reservoir temperature is 200 DEG C.
（3）The preparation of antireflection layer：After absorbed layer preparation is finished, with the Al of purity 99.99%2O3It is used as magnetic controlled sputtering target Material, controls Al2O3The Sputtering power density of target is in 6.1 W/cm-2, the air inflow of argon gas is 33 sccm during sputtering sedimentation, is adopted With rf magnetron sputtering, sputtering prepares antireflection layer, the nm of thickness 76 on absorbed layer.Absorber base reservoir temperature is in sputter procedure 200℃。
The optical property of the solar selectively absorbing coating is as follows：Under the conditions of air quality factors A M1.5, coating is inhaled Yield is 0.92, and emissivity is 0.12；Under condition of high vacuum degree, the absorptivity of coating, emissivity after 700 DEG C of long-time heat preservations Significant change does not occur.
Embodiment 2
A kind of high temperature resistant solar selectively absorbing coating, includes absorber substrate, absorbed layer and subtracts successively from bottom to surface Reflecting layer；Absorber substrate is polishing stainless steel piece, and roughness value is 0.5nm, and it is zirconium carbide and rare-earth yttrium to absorb layer material Compound, the thickness of absorbed layer compound is 300 nm.Absorbed layer compound is prepared using double target co-sputtering, and wherein zirconium carbide is adopted Prepared with DC magnetron sputtering method, rare-earth yttrium is prepared using radio frequency magnetron sputtering method；Absorbed layer compound middle rare earth yttrium is former Sub- percentage is 0.1%.Antireflection layer material is aluminum oxide, and the thickness of antireflection layer is 50 nm, and antireflection layer aluminum oxide is used Rf magnetron sputtering.
A kind of preparation method of above-mentioned high temperature resistant solar selectively absorbing coating, including following technique：
（1）The processing of absorber substrate：After the impurity that absorber substrate is removed to surface attachment, respectively in acetone and ethanol It is cleaned by ultrasonic 20 minutes respectively, nitrogen drying, vacuum is preserved；
（2）The preparation of absorbed layer：Use purity for 99.99% zirconium carbide and rare-earth yttrium as magnetic control spattering target；Using double targets Cosputtering method prepares absorbed layer, and wherein zirconium carbide uses magnetically controlled DC sputtering, and rare-earth yttrium uses radio frequency magnetron sputtering method, will Vacuum chamber takes out base vacuum to 1.0 × 10 in advance-6Torr；The Sputtering power density for adjusting zirconium carbide target is 4 W/cm-2, rare earth The Sputtering power density of yttrium target is 0.08 W/cm-2, the air inflow of argon gas is 20 sccm during sputtering sedimentation, is started in absorber The compound of depositing silicon zirconium and rare-earth yttrium in substrate, thickness is 300 nm.Absorber base reservoir temperature is 150 in sputter procedure ℃。
（3）The preparation of antireflection layer：After absorbed layer preparation is finished, with the Al of purity 99.99%2O3It is used as magnetic controlled sputtering target Material, controls Al2O3The Sputtering power density of target is in 5 W/cm-2, the air inflow of argon gas is 20 sccm during sputtering sedimentation, is used Rf magnetron sputtering sputtering on absorbed layer prepares antireflection layer, and thickness is 50 nm.Absorber base reservoir temperature is in sputter procedure 150 ℃；
The optical property of the solar selectively absorbing coating is as follows：Under the conditions of air quality factors A M1.5, coating absorptivity For 0.89, emissivity is 0.12；Under condition of high vacuum degree, the absorptivity of coating after 700 DEG C of long-time heat preservations, emissivity does not occur Significant change.
Embodiment 3
A kind of high temperature resistant solar selectively absorbing coating, includes absorber substrate, absorbed layer and subtracts successively from bottom to surface Reflecting layer；Absorber substrate is polishing stainless steel piece, and roughness value is 2 nm, and it is answering for zirconium carbide and rare-earth yttrium to absorb layer material Compound, the thickness of absorbed layer compound is 300 nm.Absorbed layer compound is prepared using double target co-sputtering, and wherein zirconium carbide is used Prepared by DC magnetron sputtering method, rare-earth yttrium is prepared using radio frequency magnetron sputtering method；Absorbed layer compound middle rare earth yttrium atom Percentage is 1%.Antireflection layer material is aluminum oxide, and the thickness of antireflection layer is 100 nm, and antireflection layer aluminum oxide uses radio frequency Magnetron sputtering.
A kind of preparation method of above-mentioned high temperature resistant solar selectively absorbing coating, including following technique：
（1）The processing of absorber substrate：After the impurity that absorber substrate is removed to surface attachment, divide respectively in acetone and ethanol Chao Shengqingxi not be 20 minutes, nitrogen drying, vacuum is preserved；
（2）The preparation of absorbed layer：Use purity for 99.99% zirconium carbide and rare-earth yttrium as magnetic control spattering target；Using double targets Cosputtering method prepares absorbed layer, and wherein zirconium carbide uses magnetically controlled DC sputtering, and rare-earth yttrium uses radio frequency magnetron sputtering method, will Vacuum chamber takes out base vacuum to 5.0 × 10 in advance-6Torr；The Sputtering power density for adjusting zirconium carbide target is 8 W/cm-2, rare earth The Sputtering power density of yttrium target is 0.3 W/cm-2, the air inflow of argon gas is 50 sccm during sputtering sedimentation, is started in absorber The compound of depositing silicon zirconium and rare-earth yttrium in substrate, thickness is 300 nm.Absorber base reservoir temperature is 250 in sputter procedure ℃。
（3）The preparation of antireflection layer：After absorbed layer preparation is finished, with the Al of purity 99.99%2O3It is used as magnetic controlled sputtering target Material, controls Al2O3The Sputtering power density of target is in 8 W/cm-2, the air inflow of argon gas is 50 sccm during sputtering sedimentation, is used Rf magnetron sputtering sputtering on absorbed layer prepares antireflection layer, the nm of thickness 100.Absorber base reservoir temperature is in sputter procedure 250 ℃。
The optical property of the solar selectively absorbing coating is as follows：Under the conditions of air quality factors A M1.5, coating is inhaled Yield is 0.88, and emissivity is 0.12；Under condition of high vacuum degree, the absorptivity of coating after 700 DEG C of long-time heat preservations, emissivity is not Generation significant change.

Claims (8)

1. a kind of high temperature resistant solar selectively absorbing coating, it is characterised in that the coating from bottom to top includes absorber base successively Bottom, absorbed layer and antireflection layer；The absorber substrate is polishing stainless steel piece, and described absorption layer material is zirconium carbide and dilute The compound of native yttrium, described antireflection layer material is aluminum oxide.
2. coating as claimed in claim 1, it is characterised in that the thickness of the absorbed layer compound is 240-300 nm.
3. coating as claimed in claim 1, it is characterised in that the atomic percent of the absorbed layer compound middle rare earth yttrium is 0.1-1%。
4. coating as claimed in claim 1, it is characterised in that the thickness of the antireflection layer is 50-100 nm.
5. coating as claimed in claim 1, it is characterised in that the polishing stainless steel piece roughness value of the absorber substrate is 0.5-2 nm。
6. the preparation method of high temperature resistant solar selectively absorbing coating as any one of claim 1 to 5, including it is following Processing step：
1）The processing of absorber substrate：After the impurity that absorber substrate is removed to surface attachment, divide respectively in acetone and ethanol Chao Shengqingxi not be 10-20 minutes, nitrogen drying, vacuum is preserved；
2）The preparation of absorbed layer：The rare-earth yttrium that purity is 99.99% for 99.99% zirconium carbide and purity is used as magnetron sputtering Target；Absorbed layer is prepared using double target co-sputtering method, wherein zirconium carbide uses magnetically controlled DC sputtering, and rare-earth yttrium uses radio-frequency magnetic Sputtering method is controlled, vacuum chamber is taken out to base vacuum in advance to 1.0 × 10-6-5.0×10-6Torr；Adjust the sputtering of zirconium carbide target Power density is 4-8 W/cm-2, the Sputtering power density of rare-earth yttrium target is 0.08-0.3 W/cm-2, argon gas during sputtering sedimentation Air inflow be 20-50 sccm, start in absorber substrate depositing silicon zirconium and rare-earth yttrium compound, thickness is 240- 300 nm；
3）The preparation of antireflection layer：After absorbed layer preparation is finished, with the Al of purity 99.99%2O3It is used as magnetic control spattering target, control Al2O3The Sputtering power density of target is in 5-8 W/cm-2, the air inflow of argon gas is 20-50 sccm during sputtering sedimentation, using penetrating The sputtering on absorbed layer of frequency magnetron sputtering prepares antireflection layer, and thickness is 50-100 nm.
7. preparation method as claimed in claim 6, it is characterised in that the step 2）Absorber in middle absorbed layer sputter procedure Base reservoir temperature is 150-250 DEG C.
8. preparation method as claimed in claim 6, it is characterised in that the step 3）Absorbed heat in middle antireflection layer sputter procedure Body base reservoir temperature is 150-250 DEG C.
CN201710289087.2A 2017-04-27 2017-04-27 A kind of high temperature resistant solar selectively absorbing coating and preparation method thereof Pending CN107190239A (en)

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Application publication date: 20170922