CN109883073B - Solar spectrum selective absorption coating with quasi-optical microcavity structure and preparation method thereof - Google Patents
Solar spectrum selective absorption coating with quasi-optical microcavity structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of material preparation, and provides a high-temperature stable solar spectrum selective absorption coating with a quasi-optical microcavity structure and a preparation method thereof. The coating comprises a metal infrared reflecting layer, a quasi-optical microcavity absorber and an optical antireflection layer from bottom to top in sequence, and the coating material contains metal W and dielectric Al2O3And SiO2The substrate is mechanically polished stainless steel 304, and is easy to prepare and obtain. The following advantages are specified with respect to the known coatings: (1) the solar absorptivity is high; (2) the high-temperature stability is good; (3) the spectral absorption range is easy to adjust and is easy for industrial application.
Description
Technical Field
The invention belongs to the technical field of material preparation, and provides a high-temperature stable solar spectrum selective absorption coating with a quasi-optical microcavity structure and a preparation method thereof.
Background
For a long time, the energy problem is particularly important, and solar energy is used as one of the alternative energy sources of the traditional energy sources, and has the advantages of cleanness, no pollution, large storage capacity and the like. The most common solar energy utilization techniques can be broadly divided into photothermal and photovoltaic. The photo-thermal technology has the advantages of high energy utilization rate, low cost, simple equipment and the like. The solar photo-thermal conversion technology is widely applied to solar water heaters, solar cooling systems and centralized solar power generation systems (CSP) by absorbing and utilizing solar energy in the form of heat energy. The solar photothermal technology is not only another utilization mode of the solar technology, but also makes up for the inherent defects of photovoltaic power generation, is suitable for the existing energy construction system, and is an effective new energy application strategy. In the photo-thermal conversion system, one of the core parts is a solar selective absorption coating, which has high absorptivity (alpha) to sunlight, and simultaneously keeps the thermal emissivity () as low as possible, and the photo-thermal conversion system has the function of absorbing the sunlight and converting the sunlight into heat energy for heating the liquid, so that the liquid is formed into a high-temperature steam to drive a motor to generate electricity, and the excellent performance of the photo-thermal conversion system is directly determined by the performance.
Solar selective absorbing coating solar selective absorbing coatings can be divided into the following six broad categories: 1) an intrinsic absorption type coating; 2) a multilayer film type absorption coating; 3) a metal-semiconductor tandem type absorption coating; 4) a surface textured absorbent coating; 5) selective transmissive and black body-like absorptive coatings; 6) cermet type absorptive coatings. In recent years, a multilayer film type selective absorption coating and a cermet type selective absorption coating have been more widely studied because of their excellent properties.
The main task of photo-thermal utilization of solar energy is to improve the photo-thermal conversion efficiency and thermal stability thereof, and the two performance indexes are directly determined by the sunlight absorptivity alpha, the thermal emissivity and the stability of the sunlight selective absorption coating. Therefore, the solar photo-thermal utilization technology mainly focuses on how to improve the solar light absorption rate α, how to reduce the thermal emissivity, and how to improve the high temperature stability thereof.
At present, the main applications of solar photo-thermal conversion technology include: solar water heater, dryer, greenhouse and solar house, solar cooker, heating and refrigerating, sea water desalting plant, solar power generation plant and high temperature solar furnace, etc. Among them, the solar water heater is the most widely applied field and the most rapidly industrialized development in solar energy utilization.
The solar photo-thermal conversion technology is mainly applied to the medium and low temperature field (400 ℃), and compared with the relatively mature low-temperature absorption coating technology, the development of the medium and high-temperature selective absorption coating faces greater challenges, for example, the optical performance of the coating is poor after the coating is recycled at high temperature, the photo-thermal conversion efficiency is low, and the like. To solve these problems, materials, structures, and manufacturing processes need to be studied and analyzed more deeply and systematically.
The selective absorbing coating of the double-layer cermet structure has been studied as already reported in patents CN102954611A, CN102653151A, CN102286720A, CN106167892A, CN103572233A, etc., with the disadvantages: with the increase of temperature, the diffusion of metal atoms in the coating can affect the optical performance of the coating, so that the absorptivity is reduced, and the emissivity is increased. Namely, there is a problem of high temperature stability and the like.
Therefore, how to improve the absorptivity of the absorption coating, reduce the emissivity of the coating and enable the coating to have good high-temperature resistance and weather resistance is a considered direction for preparing the selective absorption coating.
The main problems of the prior art include:
(1) the research is single, and mainly focuses on multilayer film type and metal ceramic type absorption coatings;
(2) the thermal stability needs to be improved;
(3) the spectral selectivity is difficult to adjust.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a high-temperature stable solar spectrum selective absorption coating with a quasi-optical microcavity structure and a preparation method thereof.
The high-temperature stable solar spectrum selective absorption coating with the quasi-optical microcavity structure can stably work in a high-temperature environment, the working temperature is 600 ℃, the solar absorption rate can reach 96 percent, the thermal emissivity can reach 5 percent, the photo-thermal conversion efficiency can reach 95 percent, and the absorption spectrum is easy to regulate and control.
Specifically, the invention is realized by the following technical proposal,
a high-temperature stable quasi-optical microcavity structure solar spectrum selective absorption coating comprises three parts: the metal infrared reflecting layer, the quasi-optical microcavity absorber and the optical antireflection layer are arranged from bottom to top in sequence,
wherein, the quasi-optical microcavity absorber is composed of a metal ceramic 1-metal ceramic 2 structure,
the metal is W, and the cermet is W-SiO2Cermet, dielectric Al of optical antireflection layer2O3And SiO2。
Among them, the metal W has a high melting point and a high reflectance in the infrared region, and is suitable as an infrared antireflection layer of the underlayer. Tong (Chinese character of 'tong')A large number of experimental researches find that the metal ceramic-metal ceramic structure is combined with absorption of metal ceramic and interaction between membrane layers, so that the metal ceramic-metal ceramic film can absorb light in a large range and has high sunlight absorption. At the same time, dielectric Al2O3And SiO2The optical constants of the layer and air are well matched, and the reflection of light can be reduced by designing the layer as an antireflection layer on the top layer. Such a choice of material layers may further optimize the solar absorption.
As a preferred technical scheme, the invention utilizes the optical constants of the single-layer film to carry out fitting optimization design through a large number of experiments to obtain the structural thickness of the film layer: the W infrared reflecting layer is about 50-150nm, W-SiO2The cermet 1 has a thickness of about 30-60nm, the intermediate metal W layer has a thickness of about 3-15nm, and W-SiO2Cermet 2 about 45-65nm, Al2O3The optical antireflection layer 1 is about 10-30nm and SiO2The optical antireflection layer 2 has a thickness of about 45 to 70 nm.
The selection of the thicknesses of the material layers is optimized by a large number of experiments, and the absorption rate of other combinations which do not select the corresponding thicknesses cannot be improved.
As a preferable embodiment of the present invention, the volume ratio of the cermet components (W: SiO)2) Is 1: 5 to 2: 3.
the material composition volume ratio is selected mainly according to the optical constant of the single-layer film, and the formed coating has good optical performance and needs good optical constant matching among the film layers. Also, if the volume ratio of the components is not properly selected, absorption will also be poor.
The invention further provides a preparation method for preparing the high-temperature stable quasi-optical microcavity structure solar spectrum selective absorption coating, which comprises the following steps:
the absorption coating is deposited from bottom to top by using mechanically polished stainless steel 304 as a substrate and a high vacuum multi-target magnetron sputtering system, wherein the metal W is deposited by direct current sputtering and has a power density of 2.00-2.50(W cm)-2)，Al2O3And SiO2By radio-frequency sputteringThe power density is 3.00-4.00(W cm)-2)，W-SiO2The metal ceramic is sequentially subjected to direct current and radio frequency co-sputtering deposition, and the sputtering power density is 0.50-1.00(W cm)-2) And 3.50-4.50(W cm)-2)。
The selection of the process parameters of the preparation method is mainly determined by combining the optical constants of the single-layer film according to the deposition power and the corresponding material deposition rate adopted during the deposition of the single-layer film. The corresponding film structure and the component ratio can be correspondingly changed according to different process parameters. The general steps of the work are to deposit a single layer film by selecting different process parameters (deposition power) and then determine the optimal process parameters through optical constants to deposit a film layer.
As a preferred technical scheme of the invention, the volume ratio of the metal ceramic components in the preparation method is (W: SiO)2) Is 1: 5 to 2: 3. w of the corresponding volume: SiO 22Is formed by sputtering and depositing two targets simultaneously by a magnetron sputtering system.
As a preferred technical scheme of the invention, the preparation method comprises the following specific preparation processes:
1) scrubbing the mechanically polished stainless steel by using acetone and absolute ethyl alcohol in sequence, and fixing a substrate;
2) vacuum pumping is carried out, the background vacuum is less than-4 × 10-4Pa；
3) Performing bias cleaning on the substrate in an argon environment at the air pressure of about 0.6-0.8Pa for 3-5 min;
4) starting sputtering, and sequentially sputtering an infrared metal W reflecting layer, a QOM quasi-optical microcavity absorbing layer and an optical antireflection layer under the argon environment and with the air pressure of about 0.3-0.5 Pa;
5) after deposition, placing in a vacuum chamber for more than 20-25min, and sampling.
The process parameters of the preparation method are selected mainly according to the deposition power and the deposition rate of corresponding materials adopted during the deposition of the single-layer film, and the optimal process parameters are determined by combining the optical constants of the single-layer film.
The high-temperature stable quasi-optical microcavity solar spectrum selective absorption coating provided by the invention has the following advantages:
(1) the solar absorptivity is high and can reach 96 percent;
(2) the high-temperature stability is good, and the performance is stable for 250 hours at the high temperature of 600 ℃ in a vacuum environment without deterioration tendency;
(3) the spectrum absorption range is easy to adjust, and the selective absorption coating based on the quasi-optical microcavity can be conveniently adjusted according to the metal component ratio, the thickness of the metal ceramic and the thickness of the middle and middle metal layers.
Drawings
FIG. 1, W-SiO of the invention stabilized at high temperature2The structure schematic diagram of the quasi-optical microcavity spectrum selective absorption coating and a reflection spectrum diagram.
Specifically, FIG. 1(a) high temperature stable W-SiO2The structure of quasi-optical microcavity selective absorbing coating is shown schematically, 1(b) the reflecting spectrum of the absorbing coating before and after annealing at 600 ℃ in vacuum environment, and 1(c) the structure is SS (substrate) \\ W \ W-SiO2\Al2O3\SiO2Reflection spectrum of sample S1, 1(d) is SS (substrate) \ W-SiO2\W\W-SiO2Reflectance spectrum of sample S2.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the invention are not limited thereto.
Example 1QOM quasi-optical microcavity based selective absorbing coating
A high-temperature stable quasi-optical microcavity structure solar spectrum selective absorption coating comprises three parts: the metal infrared reflecting layer, the quasi-optical microcavity absorber and the optical antireflection layer are arranged from bottom to top in sequence, as shown in a figure 1(a),
wherein, the quasi-optical microcavity absorber is composed of a metal ceramic 1-metal ceramic 2 structure,
the metal is W, and the cermet is W-SiO2Cermet, dielectric Al of optical antireflection layer2O3And SiO2。
Wherein the W infrared reflecting layer is about 50-150nm, W-SiO2Cermet 1 about 30-60nm with gold intermediateThe W layer is about 3-15nm, W-SiO2Cermet 2 about 45-65nm, Al2O3The optical antireflection layer 1 is about 10-30nm and SiO2The optical antireflection layer 2 has a thickness of about 45 to 70 nm. Volume ratio of cermet component (W: SiO)2) About 1: 3.
The preparation method comprises the following steps: selecting mechanically polished stainless steel 304 as substrate, and depositing the absorbing coating by using a high vacuum multi-target magnetron sputtering system, wherein the metal W is deposited by direct current sputtering with a power density of 2.00-2.50 (Wcm)-2)，Al2O3And SiO2Adopts radio frequency sputtering with power density of 3.00-4.00(W cm)-2)，W-SiO2The cermet is prepared by DC and RF co-sputtering deposition, and has sputtering power density of 0.50-1.00(W cm)-2) And 3.50-4.50(W cm)-2)。
The specific preparation process parameters are as follows:
the performance parameters of the adopted target material are as follows: the purity of each target was W (99.95%), SiO2(99.99%) and Al2O3(99.99％)。 W,SiO2And Al2O3The sizes of the targets are respectively phi 72.6mm × 5mm, phi 50.8mm × 4mm and phi 50.8mm × 4mm, and the size of the stainless steel substrate is 20 × 20mm2。
The preparation method comprises the following specific steps:
1) and scrubbing the mechanically polished stainless steel by using acetone and absolute ethyl alcohol successively, and fixing the substrate.
2) Vacuum pumping is carried out, the background vacuum is less than-4 × 10-4Pa。
3) And carrying out bias cleaning on the substrate in an argon environment at the air pressure of about 0.6-0.8Pa for 3-5 min.
4) Starting sputtering, and sputtering an infrared metal W reflecting layer, a QOM quasi-optical microcavity absorbing layer and an optical antireflection layer in sequence under the argon atmosphere and with the air pressure of about 0.3-0.5 Pa.
5) After deposition, placing in a vacuum chamber for more than 20-25min, and sampling.
Referring to the figure, FIG. 1(b) shows the reflection spectrum of the coating prepared, and the solid line is deposited W-SiO2Quasi-optical microcavityThe spectrally selective absorbing coating has no reflection spectrum measured before annealing, and the dashed curve is the reflection spectrum measured after annealing at 600 ℃ for 250 h.
Comparative example 1
S1 is SS (substrate) \\ W \ W-SiO2\Al2O3\SiO2Structural absorption coating, cermet composition and W-SiO2The quasi-optical microcavity selective absorbing coating has the same thickness as W-infrared reflecting layer of 50-150nm and W-SiO2Cermet of 90-100nm, Al2O3The optical antireflection layer 1 is about 12-17nm and SiO2The optical antireflection layer 2 has a thickness of about 58 to 62 nm.
Comparative example 2
S2 is SS \ W-SiO2\W\W-SiO2Absorption coating of structures, with W-SiO2Compared with the quasi-optical microcavity spectrum selective absorption coating, the quasi-optical microcavity spectrum selective absorption coating has no top optical antireflection layer, and the thicknesses of the layers are respectively that the W infrared reflection layer is about 100-150nm, and the W-SiO layer is2The cermet 1 has a thickness of about 30-60nm, the intermediate metal W layer has a thickness of about 2-20nm, W-SiO2The cermet 2 is about 40-65 nm.
Wherein, the S1 and S2 sample substrates are all mechanically polished stainless steel 304, and the sputtering deposition conditions are consistent with QOM quasi-optical microcavity-based selective absorbing coating.
Also, referring to the figure, the structure of 1(c) is SS \ W \ W-SiO2\Al2O3\SiO2The reflection spectrum of sample S1, 1(d) is SS \ W-SiO2\W\W-SiO2Sample S2The reflection spectrum of (1).
Example 2 comparison of Performance measurements
Under the condition of only considering normal incidence, the calculation formula of the absorptivity can be simplified as follows:
wherein λ is the wavelength; i is standard solar spectrum (AM 1.5); rλIs the emission spectrum of the corresponding wavelength. RλCan be composed of ultraviolet-visible-near infrared spectrophotometer and Fourier transform infrared spectrometerAnd (4) measuring the result. Also, considering only the normal incidence, the calculation formula of the thermal emissivity can be simplified as the following formula:
wherein M isλIs the intensity of the black body radiation at the corresponding wavelength.
The solar spectrum selective absorption coating photothermal conversion efficiency was then calculated from the absorptivity α and thermal emissivity ηThermalFollowing the following formula:
wherein σ stefan-boltzmann constant; t temperature of the coating surface; and C, the focusing multiple is the ratio of the radiation areas of the sunlight before and after focusing. If one considers the secondary conversion of thermal energy by means of a carnot heat engine, the overall efficiency of the system follows the following equation:
wherein, ηTotalIs the total efficiency after the second conversion; t is1Is ambient temperature.
Stabilizing W-SiO at high temperature according to the formula2The results of the performance calculations associated with the examples of quasi-optical microcavity spectrally selective absorbing coatings are shown in table 1:
TABLE 1W-SiO2Absorption rate, thermal emissivity, photo-thermal conversion efficiency and total system efficiency of quasi-optical microcavity spectrum selective absorption coating under different annealing conditions
The absorption of the quasi-optical microcavity selective absorbing coating is-0.96, and the thermal emissivity is-0.18 at 82 ℃. The selective absorption coating is shown to have excellent absorption performance. Meanwhile, the solar cell works at the high temperature of 600 ℃ and under the focusing environment of 1000 times, the photo-thermal conversion efficiency can reach 0.95, and the total secondary conversion efficiency can reach about 0.65.
After the coating is annealed in air at 600 ℃ for 250 hours, the change of the sunlight absorption rate is very small (0.004), the photothermal conversion efficiency can reach about 0.95 when the coating works at the working temperature of 600 ℃, and the total secondary conversion efficiency can reach about 0.65. The quasi-optical microcavity structure spectrum selective absorption coating prepared by the invention has the advantages of good high-temperature stability, high sunlight absorption rate and the like.
Comparison of S1 shows that the absorption of the QOM quasi-optical microcavity-based selective absorber coating is greater than that of the cermet type selective absorber coating by 0.96 under the same conditions. In the presence of the optical antireflective layer, the solar reflection is reduced compared to the S2 sample, which is beneficial for solar absorption by the coating.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (3)
1. A solar spectrum selective absorption coating with a quasi-optical microcavity structure is characterized by comprising three parts: the metal infrared reflecting layer, the quasi-optical microcavity absorber and the optical antireflection layer are arranged from bottom to top in sequence,
wherein, the quasi-optical microcavity absorber is composed of a metal ceramic 1-metal ceramic 2 structure,
the metal is W, and the cermet 1 is W-SiO2The metal ceramic 1 and the metal ceramic 2 are W-SiO2Cermet 2, optical anti-reflection layer of Al2O3Optical anti-reflection layer 1 and SiO2An optical antireflection layer 2;
wherein, from bottom to top are as follows: the metal W infrared reflecting layer is 50-150nm, W-SiO2The metal ceramic 1 is 30-60nm, the intermediate metal W layer is 3-15nm, and W-SiO2The cermet 2 is 45-65nm and Al2O3Optical systemThe anti-reflection layer 1 is 10-30nm of SiO2The thickness of the optical antireflection layer 2 is 45-70 nm;
and, the cermet component W: SiO 22Is 1: 5 to 2: 3.
2. a method for preparing the solar spectrum selective absorption coating of the quasi-optical microcavity structure of claim 1, comprising:
the absorption coating is deposited from bottom to top by using mechanically polished stainless steel 304 as a substrate and a high vacuum multi-target magnetron sputtering system, wherein the metal W is deposited by direct current sputtering and has a power density of 2.00-2.50(W cm)-2)，Al2O3Optical anti-reflection layer 1 and SiO2The optical antireflection layer 2 adopts radio frequency sputtering, and the power density is 3.00-4.00(W cm)-2)，W-SiO2The metal ceramic is deposited by direct current and radio frequency co-sputtering in sequence, and the sputtering power density is 0.50-1.00(W cm)-2) And 3.50-4.50(W cm)-2)。
3. The method of manufacturing according to claim 2, comprising:
1) scrubbing the mechanically polished stainless steel by using acetone and absolute ethyl alcohol in sequence, and fixing a substrate;
2) vacuumizing, wherein the background vacuum is less than 4 × 10-4Pa；
3) Performing bias cleaning on the substrate in an argon environment at the air pressure of 0.6-0.8Pa for 3-5 min;
4) starting sputtering, and sequentially sputtering an infrared metal W reflecting layer, a quasi-optical microcavity absorber and an optical antireflection layer under the argon atmosphere at the air pressure of 0.3-0.5 Pa;
5) after deposition, placing in a vacuum chamber for 20-25min, and sampling.
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| CN100457973C (en) * | 2005-10-14 | 2009-02-04 | 财团法人工业技术研究院 | Solar energy selective absorption film |
| CN102653151B (en) * | 2012-05-23 | 2015-02-11 | 皇明太阳能股份有限公司 | Solar selective absorption coating |
| CN103162452B (en) * | 2013-03-05 | 2015-04-15 | 日出东方太阳能股份有限公司 | Inoxidizability solar spectrum selective absorbing coating and preparation method thereof |
| US20170336102A1 (en) * | 2014-10-29 | 2017-11-23 | University Of Houston System | Enhanced Thermal Stability on Multi-Metal Filled Cermet Based Spectrally Selective Solar Absorbers |
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| WO2016205672A1 (en) * | 2015-06-19 | 2016-12-22 | University Of Houston System | Selective solar absorbers with tuned oxygen deficiency and methods of fabrication thereof |
| CN106468483A (en) * | 2015-08-17 | 2017-03-01 | 北京有色金属研究总院 | A kind of new stacked structure photothermal deformation coating |
| CN106167892B (en) * | 2016-08-15 | 2018-12-18 | 中国科学院宁波材料技术与工程研究所 | A kind of bimetallic/ceramic composite film and preparation method thereof |
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