CN109338297B - Hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating and preparation method thereof - Google Patents
Hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating and preparation method thereof Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- 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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- 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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- 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
Abstract
The invention provides a hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating and a preparation method thereof. The high-temperature solar energy absorption coating is composed of two layers of films, and sequentially comprises an absorption layer and an antireflection layer from the surface of the substrate upwards, wherein the absorption layer is composed of a composite ceramic film of hafnium diboride, hafnium dioxide, zirconium diboride and zirconium dioxide, and the antireflection layer is composed of aluminum oxide. The coating provided by the invention has high visible-infrared spectrum absorptivity, low infrared spectrum emissivity and good thermal stability, and the preparation process of the coating is simple and convenient, the operation is convenient, the control is easy, and the production period is shortened.
Description
Technical Field
The invention belongs to the technical field of solar thermal power generation and vacuum coating, and particularly relates to a hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating and a preparation method thereof.
Background
The solar spectrum selective absorption coating has high absorption rate in visible-near infrared bands and has a functional film with low emissivity in infrared bands, and is a key for improving the photo-thermal conversion efficiency of a solar heat collector. With the continuous development of solar heat utilization requirements and technologies, the application range of solar heat collecting pipes is developed from low-temperature application to medium-temperature application and high-temperature application, so that the use requirements of medium-high temperature application fields such as seawater desalination and solar power generation are continuously met. The selective absorption coating used for the heat collecting tube also has high-temperature thermal stability and is suitable for the service conditions of medium-high temperature environments.
The transition metal boride is a filling type ionic bond compound formed by boron (B) and transition metal (M), and the boride generally has a high melting point due to the strong covalent property of a B-B bond; and due to the existence of the M-B metal bond, the transition metal boride has the characteristics of metal materials such as high electrical conductivity, thermal conductivity and the like. The transition metal boride has excellent oxidation resistance and corrosion resistance, can work at higher temperature and in severe environment atmosphere, and has great advantages in the aspect of high-temperature structure application.
Chinese patent CN201310306881.5 discloses a solar medium-high temperature selective absorbing coating with an absorbing layer composed of boron-containing compound and a preparation method thereof. The patent utilizes a physical vapor deposition method to prepare a boron-containing compound for a selective absorption coating, introduces nitrogen and oxygen to improve the oxidation resistance and the high-temperature stability of boride, designs and prepares a multilayer gradient film system, and increases the absorption rate of a film layer.
Chinese patent CN201610824620.6 discloses a high-temperature spectral selective absorption coating based on refractory metal boride and a preparation method thereof. The solar energy absorbing coating is characterized in that the absorbing layer is made of a refractory metal boride (such as TaB) with intrinsic spectrally selective absorption characteristics and extremely excellent high temperature stability2、HfB2And ZrB2Etc.) film is the main body of spectral energy absorption by refractory metal boride and Al2O3Or SiO2The ceramic dielectric bidirectional ceramic synergizes to improve the thermal stability of the coating; and the design of a double-absorption-layer interference type film system greatly improves the spectrum selective absorption characteristic of the coating.
However, the preparation methods of the solar energy absorbing coatings related to the above two patents are complicated and not conducive to industrial production.
Disclosure of Invention
The invention aims to solve the technical problem of providing a hafnium diboride-zirconium diboride-based high-temperature solar selective absorption coating aiming at the defects in the prior art.
The invention also aims to provide a preparation method of the hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating.
A hafnium diboride-zirconium diboride-based high temperature solar energy absorption coating is characterized in that: the coating comprises an absorption layer and an antireflection layer from the surface of a substrate to the top in sequence, wherein the absorption layer is hafnium diboride HfB2Hafnium oxide HfO2Zirconium diboride ZrB2And zirconium dioxide ZrO2The composite ceramic absorption layer is obtained by magnetron sputtering hafnium diboride and zirconium diboride, wherein the hafnium diboride and the zirconium diboride are partially oxidized into hafnium dioxide and zirconium dioxide, and the antireflection layer is aluminum oxide Al2O3。
The composite ceramic absorption layer is characterized in that the thickness of the composite ceramic absorption layer is 40-120 nanometers.
The aluminum oxide of the antireflection layer is amorphous, and the thickness of the aluminum oxide is 40-150 nanometers.
The substrate is stainless steel or nickel-based alloy, and the surface roughness of the substrate is 4-8 nanometers.
The preparation method of the hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating comprises the following steps:
step 1: preparing an absorption layer, namely adopting hafnium diboride and zirconium diboride with the purity of 99.99 percent as sputtering targets, and pre-vacuumizing a vacuum chamber to 1.5 multiplied by 10-6-6.0×10-6Torr, hafnium diboride adopts a direct current magnetron sputtering technology, zirconium diboride adopts a radio frequency magnetron sputtering technology, and the hafnium diboride and the zirconium diboride are sputtered simultaneously when the absorption layer is deposited, wherein the sputtering power density of the hafnium diboride target material is 2-5W/cm-2The sputtering power density of the zirconium diboride is 3-7W/cm-2The air inflow of argon is 20-80 sccm during sputtering deposition, and an absorption layer is deposited on the substrate by using a double-target co-sputtering technology, wherein the thickness of the absorption layer is 40-120 nm;
step 2: preparing an antireflection layer, and preparing Al with the purity of 99.99 percent after the preparation of the absorption layer2O3As target material, adjusting Al2O3The sputtering power density of the target material is 4-7W/cm-2And the air inflow of argon during sputtering deposition is 20-80 sccm, and the antireflection layer is prepared on the absorption layer by sputtering by adopting radio frequency magnetron sputtering, and the thickness is 40-150 nm.
The temperature of the substrate during the preparation of the absorbing layer in the step 1 is 100-250 DEGoC。
The temperature of the substrate during the preparation of the anti-reflection layer in the step 2 is 100-250 DEGoC。
The substrate is stainless steel or nickel-based alloy, and the surface roughness of the substrate is 4-8 nanometers.
The solar selective absorption coating has the advantages that under the condition that the atmospheric quality factor AM is 1.5, the absorptivity is more than or equal to 0.90, and the emissivity is less than or equal to 0.12; under high vacuum, the mixture is passed through a filter screen 500oAnd after the coating is subjected to heat preservation for a long time, the absorptivity and emissivity of the coating are not obviously changed.
The coating of the invention adopts a double-target co-sputtering technology to prepare the composite ceramic absorption layer, and the absorption layer is hafnium diboride HfB2Hafnium oxide HfO2Zirconium diboride ZrB2And zirconium dioxide ZrO2The composite ceramic of (1). The presence of the oxide further improves the optical properties of the coating. The coating has a simple structure, is not doped, simplifies the process, is convenient to operate, shortens the production period, reduces the cost, and has wide practical value and application prospect in the fields of solar heat utilization and thermal power generation.
Drawings
FIG. 1 is a block diagram of a hafnium diboride-zirconium diboride based high temperature solar selective absorber coating of the present invention.
Detailed Description
The preparation and performance of a hafnium diboride-zirconium diboride-based high temperature solar selective absorber coating of the present invention will be further illustrated by the following specific examples.
Example 1
A preparation method of a hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating specifically comprises the following steps:
step 1: preparation of the absorbing layer: hafnium diboride and zirconium diboride with the purity of 99.99 percent are used as sputtering targets, and a vacuum chamber is pre-vacuumized to 1.5 multiplied by 10-6And (5) Torr. The hafnium diboride adopts a direct current magnetron sputtering technology, and the zirconium diboride adopts a radio frequency magnetron sputtering technology. The sputtering power density of the hafnium diboride target is adjusted to be 2W/cm-2The sputtering power density of the zirconium diboride is 3W/cm-2. The air inflow of argon during sputtering deposition is 20 sccm, and an absorption layer is deposited on a stainless steel substrate (with the roughness of 4 nanometers) by using a double-target co-sputtering technology, wherein the thickness of the absorption layer is 40 nm; during sputtering, the substrate temperature was 100 deg.CoC。
Step 2: preparing an antireflection layer: after the preparation of the absorption layer, Al with the purity of 99.99 percent is used2O3As target material, adjusting Al2O3The sputtering power density of the target material is 4W/cm-2And the air inflow of argon during sputtering deposition is 20 sccm, and the antireflection layer is prepared on the absorption layer by sputtering through radio frequency magnetron sputtering, wherein the thickness of the antireflection layer is 40 nm. During sputtering, the substrate temperature was 100 deg.CoC。
The hafnium diboride prepared by the methodThe zirconium diboride-based high-temperature solar energy absorption coating comprises an absorption layer and an antireflection layer which are sequentially arranged from the surface of a substrate upwards, wherein the substrate is a stainless steel substrate (the roughness is 4 nanometers), and the absorption layer is hafnium diboride HfB2Hafnium oxide HfO2Zirconium diboride ZrB2And zirconium dioxide ZrO2The composite ceramic absorption layer is obtained by magnetron sputtering hafnium diboride and zirconium diboride, wherein the hafnium diboride and the zirconium diboride are partially oxidized into hafnium dioxide and zirconium dioxide, and the composite ceramic thickness of the absorption layer is 40 nanometers. The antireflection layer is aluminum oxide Al2O3The alumina of the antireflection layer is amorphous and has a thickness of 40 nm.
The optical properties of the solar energy absorbing coating are as follows: under the condition of an atmospheric quality factor AM1.5, the absorptivity of the coating is 0.90, and the emissivity is 0.11.
Example 2
A preparation method of a hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating specifically comprises the following steps:
step 1: preparation of the absorbing layer: hafnium diboride and zirconium diboride with the purity of 99.99 percent are used as sputtering targets, and a vacuum chamber is pre-vacuumized to 6.0 multiplied by 10-6And (5) Torr. The hafnium diboride adopts a direct current magnetron sputtering technology, and the zirconium diboride adopts a radio frequency magnetron sputtering technology. The sputtering power density of the hafnium diboride target is adjusted to be 5W/cm-2The sputtering power density of the zirconium diboride is 7W/cm-2. The air inflow of argon during sputtering deposition is 80 sccm, and an absorption layer is deposited on a nickel-based alloy substrate (with the roughness of 8 nanometers) by using a double-target co-sputtering technology, wherein the thickness of the absorption layer is 120 nm; during sputtering, the substrate temperature was 250 deg.CoC。
Step 2: preparing an antireflection layer: after the preparation of the absorption layer, Al with the purity of 99.99 percent is used2O3As target material, adjusting Al2O3The sputtering power density of the target material is 7W/cm-2And the air inflow of argon gas during sputtering deposition is 80 sccm, and the antireflection layer is prepared on the absorption layer by sputtering through radio frequency magnetron sputtering, wherein the thickness of the antireflection layer is 150 nm. During sputtering, the substrate temperature was 250 deg.CoC。
The hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating prepared by the method sequentially comprises an absorption layer and an antireflection layer from the surface of a substrate to the top, wherein the substrate is a nickel-based alloy (with the roughness of 8 nanometers), and the absorption layer is hafnium diboride HfB2Hafnium oxide HfO2Zirconium diboride ZrB2And zirconium dioxide ZrO2The composite ceramic absorption layer is obtained by magnetron sputtering hafnium diboride and zirconium diboride, wherein the hafnium diboride and the zirconium diboride are partially oxidized into hafnium dioxide and zirconium dioxide, and the composite ceramic thickness of the absorption layer is 120 nanometers. The antireflection layer is aluminum oxide Al2O3The alumina of the antireflection layer was amorphous and had a thickness of 150 nm.
The optical properties of the solar selective absorbing coating are as follows: under the condition of an atmospheric quality factor AM1.5, the absorptivity of the coating is 0.90, and the emissivity is 0.10.
Example 3
A preparation method of a hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating specifically comprises the following steps:
step 1: preparation of the absorbing layer: hafnium diboride and zirconium diboride with the purity of 99.99 percent are used as sputtering targets, and a vacuum chamber is pre-vacuumized to 4.5 multiplied by 10-6And (5) Torr. The hafnium diboride adopts a direct current magnetron sputtering technology, and the zirconium diboride adopts a radio frequency magnetron sputtering technology. The sputtering power density of the hafnium diboride target is adjusted to be 3.8W/cm-2The sputtering power density of the zirconium diboride is 4.9W/cm-2. The air inflow of argon during sputtering deposition is 35 sccm, and an absorption layer with the thickness of 75 nm is deposited on a stainless steel substrate (with the roughness of 5 nm) by using a double-target co-sputtering technology; during sputtering, the substrate temperature was 200 deg.CoC。
Step 2: preparing an antireflection layer: after the preparation of the absorption layer, Al with the purity of 99.99 percent is used2O3As target material, adjusting Al2O3The sputtering power density of the target material is 5W/cm-2The air inflow of argon is 35 sccm during sputtering deposition, and radio frequency magnetron sputtering is adopted to prepare the antireflection film on the absorption layer by sputteringAnd the thickness of the radiation layer is 63 nm. During sputtering, the substrate temperature was 200 deg.CoC。
The hafnium diboride-zirconium diboride-based high-temperature solar energy absorption coating prepared by the method sequentially comprises an absorption layer and an antireflection layer from the surface of a substrate to the top, wherein the substrate is a stainless steel substrate (with the roughness of 5 nanometers), and the absorption layer is hafnium diboride HfB2Hafnium oxide HfO2Zirconium diboride ZrB2And zirconium dioxide ZrO2The composite ceramic absorption layer is obtained by magnetron sputtering hafnium diboride and zirconium diboride, wherein the hafnium diboride and the zirconium diboride are partially oxidized into hafnium dioxide and zirconium dioxide, and the composite ceramic thickness of the absorption layer is 120 nanometers. The antireflection layer is aluminum oxide Al2O3The alumina of the antireflection layer was amorphous and had a thickness of 150 nm.
The optical properties of the solar selective absorbing coating are as follows: under the condition of an atmospheric quality factor AM1.5, the absorptivity of the coating is 0.94, and the emissivity is 0.09.
Claims (8)
1. A hafnium diboride-zirconium diboride-based high temperature solar energy absorption coating is characterized in that: the coating comprises an absorption layer and an antireflection layer from the surface of a substrate to the top in sequence, wherein the absorption layer is hafnium diboride HfB2Hafnium oxide HfO2Zirconium diboride ZrB2And zirconium dioxide ZrO2The composite ceramic absorption layer is obtained by magnetron sputtering hafnium diboride and zirconium diboride, wherein the hafnium diboride and the zirconium diboride are partially oxidized into hafnium dioxide and zirconium dioxide, and the antireflection layer is aluminum oxide Al2O3。
2. The hafnium diboride-zirconium diboride based high temperature solar absorber coating of claim 1 wherein: the thickness of the composite ceramic absorption layer is 40-120 nanometers.
3. The hafnium diboride-zirconium diboride based high temperature solar absorber coating of claim 1 wherein: the aluminum oxide of the antireflection layer is amorphous, and the thickness of the aluminum oxide is 40-150 nanometers.
4. The hafnium diboride-zirconium diboride based high temperature solar absorber coating of claim 1 wherein: the substrate is stainless steel or nickel-based alloy, and the surface roughness of the substrate is 4-8 nanometers.
5. The preparation method of the hafnium diboride-zirconium diboride-based high temperature solar energy absorption coating according to any of the preceding claims, characterized by comprising the following steps:
step 1: preparing an absorption layer, namely adopting hafnium diboride and zirconium diboride with the purity of 99.99 percent as sputtering targets, and pre-vacuumizing a vacuum chamber to 1.5 multiplied by 10-6-6.0×10-6Torr, hafnium diboride adopts a direct current magnetron sputtering technology, zirconium diboride adopts a radio frequency magnetron sputtering technology, and the hafnium diboride and the zirconium diboride are sputtered simultaneously when the absorption layer is deposited, wherein the sputtering power density of the hafnium diboride target material is 2-5W/cm2The sputtering power density of the zirconium diboride is 3-7W/cm2The air inflow of argon is 20-80 sccm during sputtering deposition, and an absorption layer is deposited on the substrate by using a double-target co-sputtering technology, wherein the thickness of the absorption layer is 40-120 nm;
step 2: preparing an antireflection layer, and preparing Al with the purity of 99.99 percent after the preparation of the absorption layer2O3As target material, adjusting Al2O3The sputtering power density of the target material is 4-7W/cm2And the air inflow of argon during sputtering deposition is 20-80 sccm, and the antireflection layer is prepared on the absorption layer by sputtering by adopting radio frequency magnetron sputtering, and the thickness is 40-150 nm.
6. The method for preparing the hafnium diboride-zirconium diboride-based high temperature solar energy absorption coating according to claim 5, wherein the method comprises the following steps: the temperature of the substrate during the preparation of the absorbing layer in the step 1 is 100-250 ℃.
7. The method for preparing the hafnium diboride-zirconium diboride-based high temperature solar energy absorption coating according to claim 5, wherein the method comprises the following steps: the temperature of the substrate during the preparation of the anti-reflection layer in the step 2 is 100-250 ℃.
8. The method for preparing the hafnium diboride-zirconium diboride-based high temperature solar energy absorption coating according to claim 5, wherein the method comprises the following steps: the substrate is stainless steel or nickel-based alloy, and the surface roughness of the substrate is 4-8 nanometers.
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| CN110565063B (en) * | 2019-10-28 | 2020-09-08 | 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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| CN105970176B (en) * | 2016-06-15 | 2019-01-04 | 中国科学院兰州化学物理研究所 | One kind high temperature solar energy selective absorption coating containing rare-earth yttrium and preparation method thereof |
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