CN109338297A - A kind of hafnium boride-zirconium diboride high temperature solar absorber coatings and preparation method thereof - Google Patents
A kind of hafnium boride-zirconium diboride high temperature solar absorber coatings and preparation method thereof Download PDFInfo
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- CN109338297A CN109338297A CN201811244879.9A CN201811244879A CN109338297A CN 109338297 A CN109338297 A CN 109338297A CN 201811244879 A CN201811244879 A CN 201811244879A CN 109338297 A CN109338297 A CN 109338297A
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- zirconium diboride
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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
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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
- C23C14/067—Borides
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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
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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Abstract
The present invention provides a kind of hafnium boride-zirconium diboride high temperature solar absorber coatings and preparation method thereof.The high temperature solar absorber coatings are made of two membranes, it upwards successively include absorbed layer and antireflection layer from substrate surface, absorbed layer is made of the ceramic thin sheet of hafnium boride, hafnium oxide, zirconium diboride, zirconium dioxide, and antireflection layer is made of aluminium oxide.Coating provided by the invention has visible-infrared spectroscopy high-absorbility, infrared spectroscopy low-launch-rate and good thermal stability, and the preparation process of the coating is easy, easy to operate, easily controllable, the shortening production cycle.
Description
Technical field
The invention belongs to solar energy thermal-power-generatings and technical field of vacuum plating, and in particular to a kind of-two boronation of hafnium boride
Zirconium base high temperature solar absorber coatings and preparation method thereof.
Background technique
Coating for selective absorption of sunlight spectrum has high-absorbility in Visible-to-Near InfaRed wave band, has in infrared band low
The function film of emissivity is to improve the key of photothermal conversion efficiency for solar thermal collector.As solar thermal utilization needs
The application range of the continuous development of summation technology, solar energy heat collection pipe is applied from cryogenic applications to medium temperature and high temperature application development,
Constantly to meet the requirement of the high temperatures application field such as sea water desalination, solar power generation.The selection used for thermal-collecting tube
Property absorber coatings also to have a high high-temp stability, adapt to the service condition of high temperature environment.
Transition metal boride is the filled-type ion key compound that boron (B) and transition metal (M) is formed, due to B-B key
Strongly covalent property, boride generally has high-melting-point；And the presence of M-B metallic bond, transition metal boride have high conductance
The characteristic of the metal materials such as rate, thermal conductivity.Transition metal boride has excellent anti-oxidant and resistance to corrosion, can be more
It works at high temperature and rugged environment atmosphere, there is great advantage in thermal structure application aspect.
Chinese patent CN201310306881.5 discloses high in a kind of solar energy that absorbed layer is made of boron-containing compound
Temperature selective absorber coatings and preparation method thereof.The patent using physical vaporous deposition prepare boron-containing compound for selectivity
Absorber coatings, introduce nitrogen and oxygen element improves inoxidizability, improve the high-temperature stability of boride, design preparation multilayer is gradually
Become membrane system, increases the absorptivity of film layer.
Chinese patent CN201610824620.6 discloses a kind of high temperature spectrum selectivity based on refractory metal boride
Absorber coatings and preparation method.The solar energy absorbing coating is characterized in that the absorbed layer to inhale with intrinsic optical electivity
Receive refractory metal boride (such as TaB of characteristic and extremely excellent high temperature stability2、HfB2And ZrB2Deng) film be spectral energy inhale
It receives main body, pass through refractory metal boride and Al2O3Or SiO2The two-way ceramics of ceramic dielectric are synergistic, improve coating thermostabilization
Performance；And double absorption layer interference-type film structure designs, and greatly improves the optical electivity absorption characteristic of coating.
However, solar energy absorbing coating preparation method involved in above-mentioned two patent is relatively complicated, it is unfavorable for industrializing
Production.
Summary of the invention
The technical problem to be solved by the present invention is in the prior art the shortcomings that and a kind of-two boron of hafnium boride is provided
Change zirconium base high temperature solar energy selective absorption coating.
It is a further object of the present invention to provide the preparations of above-mentioned hafnium boride-zirconium diboride high temperature solar absorber coatings
Method.
A kind of hafnium boride-zirconium diboride high temperature solar absorber coatings, it is characterised in that: the coating is from substrate surface
It is followed successively by absorbed layer and antireflection layer upwards, the absorbed layer is hafnium boride HfB2, hafnium oxide HfO2, zirconium diboride ZrB2
With zirconium dioxide ZrO2Composite ceramics, the composite ceramics absorbed layer is by magnetron sputtering hafnium boride and zirconium diboride institute
, wherein hafnium boride and zirconium diboride partial oxidation are hafnium oxide and zirconium dioxide, and the antireflection layer is aluminium oxide
Al2O3。
It is characterized in that the composite ceramics absorbed layer with a thickness of 40-120 nanometers.
The aluminium oxide of the antireflection layer is amorphous state, with a thickness of 40-150 nanometers.
The substrate is stainless steel or nickel-base alloy, and the surface roughness of the substrate is 4-8 nanometers.
Above-mentioned hafnium boride-zirconium diboride high temperature solar absorber coatings preparation method, follows the steps below:
Step 1: the preparation of absorbed layer, using the hafnium boride and zirconium diboride of purity 99.99% as sputtering target material, by vacuum
Base vacuum is taken out in advance to 1.5 × 10 in room-6-6.0×10-6Torr, hafnium boride use magnetically controlled DC sputtering technology, zirconium diboride
Using radiofrequency magnetron sputtering technology, hafnium boride and zirconium diboride sputter simultaneously when deposit absorbent layer, wherein hafnium boride target
Sputtering power density be 2-5 W/cm-2, the Sputtering power density of zirconium diboride is 3-7 W/cm-2, argon gas when sputtering sedimentation
Air inflow be 20-80 sccm, using double target co-sputtering technology in substrate deposit absorbent layer, with a thickness of 40-120 nm；
Step 2: the preparation of antireflection layer, after prepared by absorbed layer, with the Al of purity 99.99%2O3As target, adjust
Al2O3The Sputtering power density of target is 4-7 W/cm-2, the air inflow of argon gas is 20-80 sccm when sputtering sedimentation, using penetrating
The sputtering on absorbed layer of frequency magnetron sputtering prepares antireflection layer, with a thickness of 40-150 nm.
Base reservoir temperature is 100-250 when in the step 1 prepared by absorbed layer oC。
Base reservoir temperature is 100-250 when in the step 2 prepared by anti-reflection layer oC。
The substrate is stainless steel or nickel-base alloy, and the surface roughness of the substrate is 4-8 nanometers.
Solar selectively absorbing coating of the invention is under the conditions of air quality factors A M1.5, absorptivity >=0.90, hair
Penetrate rate≤0.12；Under condition of high vacuum degree, through 500oAfter C long-time heat preservation, the absorptivity and emissivity of coating do not become significantly
Change.
Coating of the invention prepares composite ceramics absorbed layer using double target co-sputtering technology, and the absorbed layer is two boronations
Hafnium HfB2, hafnium oxide HfO2, zirconium diboride ZrB2With zirconium dioxide ZrO2Composite ceramics.The presence of oxide further mentions
The high optical property of coating.Coating structure of the invention is simple, does not adulterate, so that technique is simplified, it is easy to operate, shorten
Production cycle reduces cost, and the present invention is before solar thermal utilization and hot power field have wide practical value and application
Scape.
Detailed description of the invention
Fig. 1 is hafnium boride of the present invention-zirconium diboride high temperature solar energy selective absorption coating structure chart.
Specific embodiment
A kind of hafnium boride of the present invention-zirconium diboride high temperature solar energy selective is absorbed below by specific embodiment
The preparation of coating and performance are described further.
Embodiment 1
A kind of preparation method of hafnium boride-zirconium diboride high temperature solar absorber coatings, specifically follows the steps below:
Step 1: the preparation of absorbed layer: using the hafnium boride and zirconium diboride of purity 99.99% as sputtering target material, by vacuum
Base vacuum is taken out in advance to 1.5 × 10 in room-6Torr.Hafnium boride uses magnetically controlled DC sputtering technology, and zirconium diboride uses radio-frequency magnetic
Control sputtering technology.The Sputtering power density for adjusting hafnium boride target is 2 W/cm-2, the Sputtering power density of zirconium diboride is 3
W/cm-2.The air inflow of argon gas is 20 sccm when sputtering sedimentation, using double target co-sputtering technology in stainless steel base (roughness 4
Nanometer) on deposit absorbent layer, with a thickness of 40 nm；In sputtering process, base reservoir temperature 100 oC。
Step 2: the preparation of antireflection layer: after prepared by absorbed layer, with the Al of purity 99.99%2O3As target, adjust
Al2O3The Sputtering power density of target is 4 W/cm-2, the air inflow of argon gas is 20 sccm when sputtering sedimentation, using radio frequency magnetron
It sputters at sputtering on absorbed layer and prepares antireflection layer, with a thickness of 40 nm.In sputtering process, base reservoir temperature 100 oC。
Hafnium boride-zirconium diboride high temperature solar absorber coatings of above method preparation, the coating is from substrate surface
It is followed successively by absorbed layer and antireflection layer upwards, the substrate is stainless steel base (4 nanometers of roughness), and the absorbed layer is two boron
Change hafnium HfB2, hafnium oxide HfO2, zirconium diboride ZrB2With zirconium dioxide ZrO2Composite ceramics, composite ceramics absorbed layer be by
Obtained by magnetron sputtering hafnium boride and zirconium diboride, wherein hafnium boride and zirconium diboride partial oxidation are hafnium oxide and dioxy
Change zirconium, the composite ceramics of the absorbed layer are with a thickness of 40 nanometers.The antireflection layer is aluminium oxide Al2O3, the oxidation of antireflection layer
Aluminium is amorphous state, with a thickness of 40 nanometers.
The optical property of the solar energy absorbing coating is as follows: under the conditions of air quality factors A M1.5, coating absorptivity is
0.90, emissivity 0.11.
Embodiment 2
A kind of preparation method of hafnium boride-zirconium diboride high temperature solar absorber coatings, specifically follows the steps below:
Step 1: the preparation of absorbed layer: using the hafnium boride and zirconium diboride of purity 99.99% as sputtering target material, by vacuum
Base vacuum is taken out in advance to 6.0 × 10 in room-6Torr.Hafnium boride uses magnetically controlled DC sputtering technology, and zirconium diboride uses radio-frequency magnetic
Control sputtering technology.The Sputtering power density for adjusting hafnium boride target is 5 W/cm-2, the Sputtering power density of zirconium diboride is 7
W/cm-2.The air inflow of argon gas is 80 sccm when sputtering sedimentation, using double target co-sputtering technology in nickel-based alloy substrate (roughness
8 nanometers) on deposit absorbent layer, with a thickness of 120 nm；In sputtering process, base reservoir temperature 250 oC。
Step 2: the preparation of antireflection layer: after prepared by absorbed layer, with the Al of purity 99.99%2O3As target, adjust
Al2O3The Sputtering power density of target is 7 W/cm-2, the air inflow of argon gas is 80 sccm when sputtering sedimentation, using radio frequency magnetron
It sputters at sputtering on absorbed layer and prepares antireflection layer, with a thickness of 150 nm.In sputtering process, base reservoir temperature 250 oC。
Hafnium boride-zirconium diboride high temperature solar absorber coatings of above method preparation, the coating is from substrate surface
It is followed successively by absorbed layer and antireflection layer upwards, the substrate is nickel-base alloy (8 nanometers of roughness), and the absorbed layer is two boronations
Hafnium HfB2, hafnium oxide HfO2, zirconium diboride ZrB2With zirconium dioxide ZrO2Composite ceramics, composite ceramics absorbed layer is by magnetic
Obtained by control sputtering hafnium boride and zirconium diboride, wherein hafnium boride and zirconium diboride partial oxidation are hafnium oxide and titanium dioxide
Zirconium, the composite ceramics of the absorbed layer are with a thickness of 120 nanometers.The antireflection layer is aluminium oxide Al2O3, the oxygen of antireflection layer
Change aluminium is amorphous state, with a thickness of 150 nanometers.
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 0.90, emissivity 0.10.
Embodiment 3
A kind of preparation method of hafnium boride-zirconium diboride high temperature solar absorber coatings, specifically follows the steps below:
Step 1: the preparation of absorbed layer: using the hafnium boride and zirconium diboride of purity 99.99% as sputtering target material, by vacuum
Base vacuum is taken out in advance to 4.5 × 10 in room-6Torr.Hafnium boride uses magnetically controlled DC sputtering technology, and zirconium diboride uses radio-frequency magnetic
Control sputtering technology.The Sputtering power density for adjusting hafnium boride target is 3.8 W/cm-2, the Sputtering power density of zirconium diboride is
4.9 W/cm-2.The air inflow of argon gas is 35 sccm when sputtering sedimentation, (coarse in stainless steel base using double target co-sputtering technology
Degree 5 nanometers) on deposit absorbent layer, with a thickness of 75 nm；In sputtering process, base reservoir temperature 200 oC。
Step 2: the preparation of antireflection layer: after prepared by absorbed layer, with the Al of purity 99.99%2O3As target, adjust
Al2O3The Sputtering power density of target is 5 W/cm-2, the air inflow of argon gas is 35 sccm when sputtering sedimentation, using radio frequency magnetron
It sputters at sputtering on absorbed layer and prepares antireflection layer, with a thickness of 63 nm.In sputtering process, base reservoir temperature 200 oC。
Hafnium boride-zirconium diboride high temperature solar absorber coatings of above method preparation, the coating is from substrate surface
It is followed successively by absorbed layer and antireflection layer upwards, the substrate is stainless steel base (5 nanometers of roughness), and the absorbed layer is two boron
Change hafnium HfB2, hafnium oxide HfO2, zirconium diboride ZrB2With zirconium dioxide ZrO2Composite ceramics, composite ceramics absorbed layer be by
Obtained by magnetron sputtering hafnium boride and zirconium diboride, wherein hafnium boride and zirconium diboride partial oxidation are hafnium oxide and dioxy
Change zirconium, the composite ceramics of the absorbed layer are with a thickness of 120 nanometers.The antireflection layer is aluminium oxide Al2O3, antireflection layer
Aluminium oxide is amorphous state, with a thickness of 150 nanometers.
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 0.94, emissivity 0.09.
Claims (8)
1. a kind of hafnium boride-zirconium diboride high temperature solar absorber coatings, it is characterised in that: the coating from substrate surface to
On be followed successively by absorbed layer and antireflection layer, the absorbed layer is hafnium boride HfB2, hafnium oxide HfO2, zirconium diboride ZrB2With
Zirconium dioxide ZrO2Composite ceramics, the composite ceramics absorbed layer be obtained by magnetron sputtering hafnium boride and zirconium diboride,
Wherein hafnium boride and zirconium diboride partial oxidation are hafnium oxide and zirconium dioxide, and the antireflection layer is aluminium oxide
Al2O3。
2. a kind of hafnium boride according to claim 1-zirconium diboride high temperature solar absorber coatings, feature exist
In: the composite ceramics absorbed layer with a thickness of 40-120 nanometers.
3. a kind of hafnium boride according to claim 1-zirconium diboride high temperature solar absorber coatings, feature exist
In: the aluminium oxide of the antireflection layer is amorphous state, with a thickness of 40-150 nanometers.
4. a kind of hafnium boride according to claim 1-zirconium diboride high temperature solar absorber coatings, feature exist
In: the substrate is stainless steel or nickel-base alloy, and the surface roughness of the substrate is 4-8 nanometers.
5. a kind of preparation side of hafnium boride-zirconium diboride high temperature solar absorber coatings described in above-mentioned any claim
Method, it is characterised in that follow the steps below:
Step 1: the preparation of absorbed layer, using the hafnium boride and zirconium diboride of purity 99.99% as sputtering target material, by vacuum
Base vacuum is taken out in advance to 1.5 × 10 in room-6-6.0×10-6Torr, hafnium boride use magnetically controlled DC sputtering technology, zirconium diboride
Using radiofrequency magnetron sputtering technology, hafnium boride and zirconium diboride sputter simultaneously when deposit absorbent layer, wherein hafnium boride target
Sputtering power density be 2-5 W/cm-2, the Sputtering power density of zirconium diboride is 3-7 W/cm-2, argon gas when sputtering sedimentation
Air inflow be 20-80 sccm, using double target co-sputtering technology in substrate deposit absorbent layer, with a thickness of 40-120 nm；
Step 2: the preparation of antireflection layer, after prepared by absorbed layer, with the Al of purity 99.99%2O3As target, Al is adjusted2O3
The Sputtering power density of target is 4-7 W/cm-2, the air inflow of argon gas is 20-80 sccm when sputtering sedimentation, using radio frequency magnetron
It sputters at sputtering on absorbed layer and prepares antireflection layer, with a thickness of 40-150 nm.
6. a kind of hafnium boride according to claim 5-zirconium diboride high temperature solar absorber coatings preparation method,
It is characterized by: base reservoir temperature is 100-250 when in the step 1 prepared by absorbed layeroC。
7. a kind of hafnium boride according to claim 5-zirconium diboride high temperature solar absorber coatings preparation method,
It is characterized by: base reservoir temperature is 100-250 when in the step 2 prepared by anti-reflection layeroC。
8. a kind of hafnium boride according to claim 5-zirconium diboride high temperature solar absorber coatings preparation method,
It is characterized by: the substrate is stainless steel or nickel-base alloy, the surface roughness of the substrate is 4-8 nanometers.
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| CN110565063A (en) * | 2019-10-28 | 2019-12-13 | 吉林大学 | Zirconium tantalum boron coating and preparation method and application thereof |
| CN111321382A (en) * | 2020-03-03 | 2020-06-23 | 电子科技大学 | High-temperature-resistant and oxidation-resistant infrared low-emissivity composite film and preparation method thereof |
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| CN110565063A (en) * | 2019-10-28 | 2019-12-13 | 吉林大学 | Zirconium tantalum boron coating and preparation method and application thereof |
| CN111321382A (en) * | 2020-03-03 | 2020-06-23 | 电子科技大学 | High-temperature-resistant and oxidation-resistant infrared low-emissivity composite film and preparation method thereof |
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