CN114959581A - Preparation method of solar spectrum absorption coating and coating - Google Patents
Preparation method of solar spectrum absorption coating and coating Download PDFInfo
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- CN114959581A CN114959581A CN202210265585.4A CN202210265585A CN114959581A CN 114959581 A CN114959581 A CN 114959581A CN 202210265585 A CN202210265585 A CN 202210265585A CN 114959581 A CN114959581 A CN 114959581A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 135
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 67
- 238000001228 spectrum Methods 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 40
- 239000000956 alloy Substances 0.000 claims abstract description 40
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 229910002064 alloy oxide Inorganic materials 0.000 claims abstract description 36
- 150000004767 nitrides Chemical class 0.000 claims abstract description 30
- 238000000151 deposition Methods 0.000 claims abstract description 29
- 231100000572 poisoning Toxicity 0.000 claims abstract description 26
- 230000000607 poisoning effect Effects 0.000 claims abstract description 26
- 230000008021 deposition Effects 0.000 claims abstract description 25
- 239000013077 target material Substances 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 21
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- KZNMRPQBBZBTSW-UHFFFAOYSA-N [Au]=O Chemical compound [Au]=O KZNMRPQBBZBTSW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910001922 gold oxide Inorganic materials 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
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- 241000196324 Embryophyta Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0084—Producing gradient compositions
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C23C14/0089—Reactive sputtering in metallic mode
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/08—Oxides
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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
- C23C14/14—Metallic material, boron or silicon
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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
- C23C14/14—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
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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
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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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/225—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption for spectrally selective absorption
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/25—Coatings made of metallic material
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/40—Solar thermal energy, e.g. solar towers
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Abstract
The invention discloses a preparation method of a solar spectrum absorption coating and the coating, comprising the following steps: mounting a target, a substrate and a protective screen between the target and the substrate in sputtering equipment, adjusting the vacuum degree and the temperature of the sputtering equipment to target values, introducing inert gas, and generating plasma; introducing mixed gas flow of oxygen/nitrogen and inert gas, removing the protective screen, and performing pure gold deposition on the substrate; gradually generating target poisoning on the target material along with the deposition, and continuing to deposit a mixture comprising a large amount of alloy and a small amount of alloy oxide/nitride on the substrate; as the deposition continues, the target becomes more poisoned, depositing a mixture comprising a small amount of alloy and a large amount of alloy oxide/nitride on the substrate; finally, the target material is completely poisoned, and pure gold oxide/nitride is deposited on the substrate to obtain the required solar spectrum absorption layer. The invention has low cost, integral coating, great spectrum absorption potential, high heat stability and good oxidation resistance.
Description
Technical Field
The invention belongs to the technical field of coating preparation, and particularly relates to a preparation method of a solar spectrum absorption coating and the coating.
Background
Solar energy is a clean, green, free and renewable energy source, almost worldwide. The most environment-friendly and efficient technology for developing and utilizing solar energy is a solar photo-thermal conversion system, which is called a concentrating solar system (CSP). Concentrating solar systems have shown great application prospects and are currently being deployed worldwide, with 7% of the global power being expected to be generated by 2030 and up to 25% by 2050. CSP systems generally consist of a heat collector, a receiver, a heat transfer fluid, a thermal energy store, etc., and convert solar energy to thermal energy by means of a Solar Selective Absorber Coating (SSACs) deposited on the receiver, so that the performance of the SSACs determines the efficiency of the photothermal conversion. However, the higher the temperature of the heat transfer fluid, the higher the Carnot thermal efficiency of the power plant
The higher the roadmap of the next generation CSP plant, the more than 650 ℃ the operating temperature of the central tower is expected to be, and the operating temperature of the solar fieldFrom 400 ℃ to over 500 ℃. In order to achieve a high spectral selectivity of the coating, the coating is required to:
absorbing as much sunlight as possible in the solar radiation range, i.e., in the ultraviolet-visible-near infrared band (0.3-2.5 μm) (absorption α is 1, reflectance R is 0);
secondly, the black body heat radiation epsilon is released as little as possible in an infrared range (more than 2.5 mu m);
and thirdly, the heat stability of more than 600 ℃ and even higher, and the property of enduring long-term exposure to moisture and other environmental conditions.
② when the solar energy absorbing coating works in the temperature range of 400-.
Overall, therefore, an ideal solar spectrum absorbing coating should be ideally black in the uv-vis-nir band (0.3-2.5 μm, corresponding to the full band of the solar spectrum), i.e. with an absorption α of 1 and a reflectance R of 0; in the infrared range (greater than 2.5 μm, without solar radiation) the mirror is ideal, i.e. the absorption α ═ e ═ 0 and the reflection R ═ 1.
And thus can be achieved by using materials with high thermal conductivity, low coefficient of expansion, low refractive index, oxidation resistance. Mainly on the thermal and structural stability of the individual and combined layers, good adhesion between the substrate and the adjacent layers and an increased resistance to thermal and mechanical stresses.
Since the SSAC concept was proposed by Tabor in the 50's of the last century, the preparation and design of coatings has received extensive attention. Since it is difficult for the monolayer to achieve maximum absorbance, the spectral selectivity of the SSAC can be optimized by changing the structure of the coating, selecting different materials or deposition methods.
(1) Changing the structure of the absorption coating: the coating is improved from a single-layer structure to a multi-layer interference layer coating, each layer in the coating can be made of metal, dielectric or metal dielectric composite materials, the absorption is realized near the solar radiation peak value by utilizing the interference effect of light, the absorption is not realized in an infrared band, and the high infrared reflection characteristic of the substrate is corresponded. Secondly, designing a selective solar absorber with a multilayer structure, wherein the absorber consists of three layers of high-reflection metal substrates, the first layer on a substrate is an absorption layer, the absorption layer consists of high-concentration metal particles in a medium matrix and is called a High Metal Volume Fraction (HMVF) layer, the second absorption layer has lower metal concentration and is called a Low Metal Volume Fraction (LMVF) layer, the HMVF and the LMVF are homogeneous ceramic layers, the uppermost third layer is made of a medium material with low refractive index n, and the surface reflection is inhibited in a visible range, namely the layer has the function of an anti-reflection coating. However, the absorption coating with a multilayer structure has strict requirements on the manufacturing process and the manufacturing precision, different targets need to be prepared and independent process parameters need to be set for each layer, the performance of each layer also needs to be measured and controlled independently, and the method is long in time consumption, high in cost, high in preparation difficulty and low in repeatability.
Selecting a material with better physical properties: the better performance is a bimetallic ceramic coating, a transition metal carbide and nitride coating, a high temperature transition metal oxide coating, etc., but does not provide more possibilities in solar photo-thermal conversion applications. Metal doped Al such as Ag, Mo, W, Ni 2 O 3 、AlN、SiO 2 And AlSiO x Bimetallic ceramic coating, HfC, TiC, TiN, ZrN transition metal carbide and nitride, CrN/CrOD/CrOM/SiO 2 And CrAlO-based and other transition metal oxide coatings obtain more valuable results, and have wide commercial application at the temperature of below 400 ℃, but at higher temperature, the coatings have defects of holes, cracks, boundary widening and the like due to nanoparticle recombination, element diffusion and phase change, and even fall off, the thermal emissivity of the coatings is increased, the absorptivity is reduced, and the thermal stability still can not meet the requirements of a new generation of CSP.
Disclosure of Invention
The invention aims to provide a preparation method of a solar spectrum absorption coating aiming at the defects of the prior art, the method is simple in process and low in cost, and the prepared coating is integrally formed, has great spectrum absorption potential, high thermal stability and good oxidation resistance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a solar spectrum absorption coating comprises the following steps:
step 1: installing a target material, a substrate and a protective screen between the target material and the substrate in sputtering equipment, adjusting the vacuum degree and the temperature of the sputtering equipment to target values, introducing inert gas, and generating plasma at the moment;
step 2: introducing mixed gas flow of oxygen and inert gas or mixed gas flow of nitrogen and inert gas, removing the protective screen, and primarily performing pure gold deposition on the substrate;
and step 3: gradually generating target poisoning on the target along with the progress of deposition, generating a poisoning layer on the surface of the target, continuing the deposition, and depositing a mixture comprising a large amount of alloy and a small amount of alloy oxide/nitride on the substrate;
and 4, step 4: as the deposition continues, the poisoning degree of the target material is deepened, a mixture comprising a small amount of alloy and a large amount of alloy oxide/nitride is deposited on the substrate, the deposition is continued until the target material is completely poisoned, and pure gold oxide/nitride is deposited on the substrate, so that the required solar spectrum absorption layer with a gradual change and gradient structure is obtained.
Preferably, the steps are continued, and a layer of pure gold oxide and nitride is further deposited on the surface of the prepared gradient coating to be used as an anti-reflection layer, so that the preparation of the solar spectrum absorption coating containing the absorption layer and the anti-reflection layer is completed.
Preferably, in step 1, the vacuum is less than 10 -3 Pa, temperature between 100 ℃ and 300 ℃.
Preferably, the flow rate of the mixed gas stream in step 2 is generally between 1.5 and 5Pa, and the ratio of oxygen to inert gas/nitrogen to inert gas is between 0 and 1.
Preferably, the target material is a high-entropy alloy.
Another object of the present invention is to provide a solar-spectrum absorbing coating obtained according to the above method for preparing a solar-spectrum absorbing coating.
Preferably, the reflectivity of the solar spectrum absorption coating of the gradient high-entropy alloy is not higher than 0.02 and the light absorptivity alpha is not lower than 0.95 in a wave band of 0.3-2.5 μm, the heat radiation epsilon is not higher than 0.095 in a wave band of higher than 2.5 μm, and the spectrum absorption selectivity alpha/epsilon is higher than 10.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the solar spectrum absorption coating provided by the invention has the advantages of low cost, low requirement on equipment, simplicity and convenience in operation and short time consumption, the prepared solar spectrum absorption coating has a metal component gradient structure, the farther away the solar spectrum absorption coating is from a substrate, the lower the metal content is, the part in contact with the substrate is pure high-entropy alloy, the surface part of the coating is pure high-entropy oxide/nitride with high oxidation resistance and high temperature resistance, and the problem of large brittleness and cracking of the conventional SSACs coating is solved; the surface part of the coating is pure high-entropy oxide/nitride with high oxidation resistance and high temperature resistance, and the coating has the advantages of oxidation resistance, high temperature resistance and high absorption ratio, and meets the requirements of a new generation of CSP technology;
(2) the coating prepared by the invention has an integrated structure, comprises all structural layers (the infrared metal mirror, the metal-rich absorption layer, the oxide-rich absorption layer and the anti-reflection oxidation layer), can be formed in one process step, does not need to design different targets and parameters aiming at different functions of each structural layer, and can prepare the whole coating by using the same target material, gas supply and other process parameters; this shows that, on the one hand, the invention reduces the number of parameters to be set, can better control the manufacture of the solar energy absorbing layer, and in addition, the preparation speed is faster, which is beneficial to improving the repeatability of the optical performance and the productivity of the device;
(3) the prepared coating has great spectrum absorption potential, the reflectivity of the prepared coating can be effectively reduced to 0.004 in a visible light wave band, the light absorption rate reaches 0.98, and the absorption ratio reaches 16.3; the reflectivity spectrum of the coating is almost unchanged before annealing at 550 ℃ for 20h, the light absorptivity alpha of the coating is stabilized at 0.96 in a solar spectrum waveband (0.3-2.5 mu m), and the thermal radiance epsilon of the coating is stabilized at 0.09 in an infrared waveband higher than 2.5 mu m, which shows that the coating has good high-temperature stability; the novel structural coating with gradually changed components is expected to replace the traditional double-layer and multi-layer solar spectrum absorption coating, and has huge engineering application potential;
(4) the preparation method of the solar spectrum absorption coating provided by the invention is not only suitable for the high-entropy alloy heat absorption coating, but also can be used for preparing other functional coatings, and the corresponding component gradient coating can be prepared only by selecting appropriate target materials and parameters according to the application and performance requirements of a target coating, so that the application field is wide.
(5) Compared with other solar spectrum absorbing materials, the solar spectrum absorbing coating has the advantages of performance, the high-entropy alloy is used as the target material, has high-entropy effect in thermodynamics and slow diffusion effect in kinetics, and has high-temperature resistance and oxidation resistance compared with conventional ternary and quaternary nitride and oxide coatings; and the oxygen/nitrogen is doped to form highly stable high-entropy alloy oxide/nitride on the surface of the coating, so that the high-temperature oxidation resistance of the coating is further improved, and the light absorption performance of the coating cannot be influenced even if the temperature and the oxygen content in the SSACs are greatly fluctuated in the using process.
Drawings
FIG. 1 is a schematic diagram of the steps of a method for preparing a solar spectrum absorption coating according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a solar spectrum absorption coating according to an embodiment of the present invention;
FIG. 3 is an image of a cross-sectional structure of HRTEM of the novel high-entropy alloy heat-absorbing coating structure with gradually changed compositions in the second embodiment of the present invention;
FIG. 4 is the measured reflectance of the AlCrNbSiTaTiYO new high-entropy alloy heat-absorbing coating with gradually changed composition in the second embodiment of the present invention at the full spectrum band;
FIG. 5 shows the measured reflectance of the AlCrNbSiTiO novel high-entropy alloy heat-absorbing coating with gradually changed components before and after annealing in the third embodiment of the present invention at the full spectrum band;
wherein, in fig. 1: 1-target, 2-substrate, 3-shield, 4-pure Ar gas flow, 5-plasma (blue), 5' -plasma (violet), 5 "-plasma (rose), 6-O 2 a/Ar mixed gas flow, 7-deposited coating (early), 7' -deposited coating (medium), 7 "-deposited coating (late), 8-poisoned layer, 9-anti-reflective layer;
in fig. 2: 10-substrate, 11-pure alloy coating, 12-alloy + alloy oxide coating and 13-pure oxide coating;
in fig. 3: 14-Cu substrate, 15-pure high-entropy alloy coating, 16-high-entropy alloy and high-entropy alloy oxide coating, and 17-pure high-entropy alloy oxide coating;
in fig. 4: 18-component gradient AlCrNbSiTaTiYO high-entropy alloy oxide coating reflectivity map, 19-traditional structure absorption coating reflectivity map, and 20-ideal solar spectrum absorption coating reflectivity map;
in fig. 5: 21-a reflectivity map of the AlCrNbSiTiO high-entropy alloy oxide coating with gradually changed components before annealing, 22-550 ℃, 5h of the AlCrNbSiTiO high-entropy alloy oxide coating with gradually changed components after annealing, and 23-550 ℃, 20h of the AlCrNbSiTiO high-entropy alloy oxide coating with gradually changed components after annealing.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
The invention provides a preparation method of a solar spectrum absorption coating, which comprises the following steps:
(1) on a radio frequency magnetron sputtering PVD device, a target material, a substrate and a protective screen between the target material and the substrate which are placed oppositely are installed, the vacuum degree is adjusted to an ideal value, the temperature is adjusted to a target value, high-purity Ar gas is introduced, and at the moment, blue plasma is generated;
(2) introduction of O 2 /Ar or N 2 a/Ar mixed gas flow while removing the shield, the plasma still being blue, meaning that only pure gold deposition occurs in the initial stage, a dark deposit (infrared metal mirror) appearing on the substrate;
(3) as the deposition progresses, the target material gradually generates target poisoning, and a poisoning layer (if O is introduced) appears on the surface of the target material 2 In the case of Ar gas flow, the poisoning layer is an oxide layer, if N is introduced 2 the/Ar gas flow, the poisoning layer is a nitriding layer), and the plasma slowly turns purple, and then slowly enters the middle deposition period, the deposited coating is not pure alloy any more, but a mixture (metal-rich absorption layer) consisting of a large amount of alloy and a small amount of alloy oxide/nitride, and the color of the coating gradually becomes lighter;
(4) the target poisoning degree is deepened along with the continuous progress of deposition, the plasma is gradually changed into rosy, and then the deposition later stage is carried out, the deposited coating is a mixture consisting of a small amount of alloy and a large amount of alloy oxide/nitride, the color of the coating is further lightened, and the coating is finally deposited to be transparent pure gold oxide (an oxide/nitride-rich absorption layer);
(5) in order to improve the reflection performance of the coating, a layer of pure gold oxide/nitride is further deposited to be used as an anti-reflection layer, and the preparation of the ideal solar spectrum absorption coating containing an absorption layer and the anti-reflection layer is completed.
The target material and the substrate are determined by the purpose and the performance of the target coating, high-entropy alloy can be selected as the target material, and the protective screen can be made of stainless steel materials and used for blocking and isolating a sample and preventing an impurity layer from being generated on the substrate before oxygen or nitrogen is introduced. The vacuum degree is generally less than 10 -3 Pa, the temperature in the sputtering equipment is determined by the coating application and performance, and is generally between 100 ℃ and 300 ℃. O is 2 Ar or N 2 The flow rate of the/Ar mixed gas flow is generally 1.5-5Pa, O 2 /Ar or N 2 the/Ar ratio is between 0 and 1. Ar is used for bombarding the target material and sputtering the target material, O 2 /N 2 For oxidizing or nitriding the sputtering product, causing target poisoning phenomena, so that the deposited coating is an oxide or nitride.
Target poisoning refers to the introduction of reactive gas O during the sputtering process 2 Or N 2 And generating chemical reaction with the target surface atoms to generate oxide or nitride, so that the sputtering channel on the target surface is covered by the generated matter. The target poisoning degree is realized by regulating and controlling the flow rate and the target temperature of the reaction gas.
The deposition process (taking the example that the product of target poisoning is oxide), since target poisoning has a hysteresis effect, target poisoning has not yet started in the initial stage, the sputtering is pure gold, the plasma is blue, and the deposited coating is made of 100% alloy; following the interior of the chamber O 2 The content is increased to a certain degree, target poisoning occurs, and the surface of the target part is covered with a layer of thin oxide, Ar + A small amount of alloy oxide can be sputtered while the alloy is stripped, and the plasma is purple, so that the deposit is not pure alloy any more; as the poisoning degree of the target deepens, the oxide generation rate is higher than the stripping rate of the target, the wider the coverage area and the larger the thickness of the product poisoned by the target are, the oxide proportion in the sputtering product gradually increases, and the metal component of the deposit continuously and gradually decreases; until the whole target material is covered by the alloy oxide and the target is completely poisoned, at the end of deposition, only the alloy oxide exists in the sputtering product, and the plasma is rosy, so that the deposition is only composed of 100% of the alloy oxide; the further away from the substrate the lower the metal content of the coating for the entire deposition process.
The anti-reflection layer is made of pure gold oxide, surface reflection is inhibited, the reflectivity in a wave band of 0.3-2.5 microns can be effectively reduced, the spectral selectivity is improved, meanwhile, the high-entropy alloy oxide/nitride with high stability further improves the oxidation capacity of the coating, and the light absorption performance of the coating cannot be influenced even if the oxygen content in the SSACs fluctuates greatly in the using process.
The plasma is a mixture of sputtering products and bombarding ions, the color of which depends on the ion species and the ratio of the ions, for example, the sputtering products are only alloys in the early stage of sputtering, the plasma is blue, the color is uniformly transited to purple with the addition of oxides, and the sputtering products are only alloy oxides in the end stage of sputtering, so the plasma is rosy.
The coating measurements were HRTEM cross-sectional measurements to analyze the composition gradient structure. The optical performance is characterized by testing through a spectrophotometer and a Fourier spectrometer, the optical performance is characterized in that the reflectivity R of the coating with the thickness of 0.25-2.5 mu m is measured in a full spectrum wave band, and then the absorptivity alpha in a solar spectrum wave band, the self thermal radiance epsilon in an infrared wave band and the spectrum absorption selectivity alpha/epsilon are respectively calculated.
Conversion formula of absorption rate and reflectivity of the coating in the solar spectrum band (0.3-2.5 μm):
the conversion formula of the emissivity and the reflectivity of the coating in an infrared band (2.5-25 mu m) is as follows:
in the above formula, R, α, and ∈ are respectively the reflectance, the absorbance, and the thermal emissivity, and it can be seen that the higher the reflectance R, the lower the coating absorbance and the thermal emissivity.
The invention is further illustrated by the following specific examples.
The first embodiment is as follows:
taking the preparation of a high-entropy alloy oxide coating as an example, the invention provides a preparation method of a gradient high-entropy alloy solar spectrum absorption coating, which comprises the following steps:
(1) referring to fig. 1(a), in a PVD apparatus, a target 1, a substrate 2, and a shield 3 between the target 1 and the substrate 2 are installed in a state where a degree of vacuum is 10 -3 Pa, when the temperature reaches 150 ℃, introducing high-purity Ar gas 4, and then producingBlue-producing plasma 5;
(2) referring to FIG. 1(b), O is introduced 2 Removing the protective shield 3 while the/Ar mixed gas flow 6 is flowing, the plasma still being blue, meaning that an initial pure gold deposition has occurred and a dark deposit 7 on the substrate has occurred;
(3) referring to fig. 1(c), as the deposition progresses, the target poisoning gradually occurs on the target, the poisoning layer 8 appears on the surface of the target, the plasma slowly changes to purple 5 ', at the moment, the deposition medium stage is entered, the deposited coating is not pure alloy any more, but is a mixture 7' of a large amount of alloy and a small amount of alloy oxide, and the color gradually becomes lighter;
(4) referring to fig. 1(d), as the deposition progresses, the target poisoning degree increases, the plasma gradually turns to rosy 5 ", and then the deposition later stage is entered, the deposited coating is a mixture 7" of a small amount of alloy and a large amount of alloy oxide, so that the color is further gradually lightened, and finally, the transparent pure gold oxide is obtained;
(5) referring to fig. 1(e), in order to improve the reflective performance of the coating, a layer of pure gold oxide is further deposited as an anti-reflection layer 9, and the preparation of the solar energy absorption coating is completed.
Target poisoning refers to the introduction of reactive gas O during the sputtering process 2 Or N 2 And (3) generating chemical reaction with target surface atoms to generate oxide or nitride 8, so that the sputtering channel on the target surface is covered by the generated matter. The target poisoning degree is realized by regulating and controlling the flow rate of the reaction gas and the target temperature.
Target poisoning is a gentle process, which is characterized in that the color of plasma is slowly converted from blue 5 to purple 5 'and then gradually changed to rose 5', which means that the plasma is uniform and gradual change of the metal content in the deposited coating, the blue is pure alloy, the rose is pure oxide, namely the coating firstly deposits the pure alloy, then the alloy components are gradually and uniformly reduced, the alloy and the alloy oxide are deposited, and finally the alloy components are zero, and the gold oxide is deposited.
The anti-reflection layer is made of pure gold oxide, so that the reflectivity in a wave band of 0.3-2.5 microns can be effectively reduced, the spectral selectivity is improved, meanwhile, the high-entropy alloy oxide/nitride with high stability further improves the oxidation capacity of the coating, and the light absorption performance of the coating cannot be influenced even if the oxygen content in the SSACs fluctuates greatly in the using process.
The coating measurements were HRTEM cross-sectional measurements to analyze the composition gradient structure.
The optical performance is characterized by testing through a spectrophotometer and a Fourier spectrometer, and is characterized in that the reflectivity R of the coating with the thickness of 0.25-2.5 mu m is measured in a full spectrum wave band, the absorptivity alpha in a solar spectrum wave band is calculated through a formula (1), the self-heat radiance epsilon in an infrared wave band is calculated through a formula (2), and the spectrum absorption selectivity alpha/epsilon is calculated.
The sectional structure image of the resulting coating HRTEM is shown in fig. 2, and comprises an absorption layer and an anti-reflection layer 13, wherein the absorption layer is different from a conventional two-layer or multi-layer model, but has an integral structure, is uniformly transited from a pure alloy 11 to an alloy oxide/nitride 12, has a distinct composition gradient structure, and is then deposited with a layer of pure gold oxide/nitride as the anti-reflection layer 13.
Example two:
taking the preparation of AlCrNbSiTaTiYO high entropy alloy oxide coating with gradually changed components as an example. Selecting a Cu substrate and an AlCrNbSiTaTiY high-entropy alloy target (Al: Cr: Nb: Si: Ta: Ti: Y: 25:20:20:15:5:10:5), introducing O at the temperature of 150 ℃ in a cavity 2 The flow rate of the/Ar mixed gas flow is 1.5Pa, O 2 Ar is 1:10, and after 2min, a HRTEM image of the cross section of the coating is obtained as shown in FIG. 3, which comprises a 70nm thick absorption layer and a 50nm anti-reflection layer 17, wherein the absorption layer has an integral structure, is about 10nm thick from a pure alloy 15 and then is uniformly transited to an alloy oxide/nitride 16, and the composition gradient layer is about 60 nm.
The measured reflection spectrum is shown in figure 4, the reflectivity spectrum 18 of the AlCrNbSiTaTiYO high-entropy alloy oxide coating with the novel structure with gradually-changed components is superior to the reflectivity spectrum 19 of the absorption coating with the traditional structure and is closer to the reflectivity spectrum 20 of the absorption coating with the ideal solar spectrum, and the spectrum absorption selectivity ratios alpha/epsilon of 18 and 19 are respectively 16.3 and 9.2:
firstly, in a solar spectrum wave band smaller than 1.8 mu m, the reflectivity R of a curve 18 is as low as 0.004, the light absorptivity alpha is as high as 0.98, the absorption ratio is as high as 16, the curve is stable, the reflectivity of a curve 19 has volatility and is obviously higher than 18, particularly in a visible light wave band, the reflectivity R of the curve 19 is as high as 0.12, and the light absorptivity alpha is only 0.92, which shows that in a low wavelength wave band, the high-entropy alloy oxide coating with the gradually-changed novel structure has more stable and lower reflectivity value, namely, the absorptivity is higher than that of an absorption coating with a traditional structure.
Secondly, in an infrared band higher than 1.8 mu m, the curve 18 is higher than the curve 19, the reflectivity R of the curve 18 is up to 96 percent, the thermal emissivity epsilon is only 0.06, the reflectivity R of the curve 19 is about 0.89, and the thermal emissivity epsilon is about 0.1, which means that the high-entropy alloy oxide coating with the gradually-changed novel structure has lower thermal radiation in the infrared band and higher energy utilization rate.
Example three:
taking the preparation of AlCrNbSiTiO high entropy alloy oxide coating with gradually changed components as an example. Selecting a stainless steel substrate wrapped by a Mo coating and an AlCrNbSiTi high-entropy alloy target (Al: Cr: Nb: Si: Ti: 34:20:13:11:22), introducing O at the temperature of 100 ℃ in a cavity 2 The flow rate of the/Ar mixed gas flow is 1.5Pa, O 2 Ar is 1:10, after 2.5min, the obtained coating has the thickness of 250nm, comprises an absorption layer with the thickness of 200nm and a 50nm anti-reflection layer, the absorption layer has an integral structure, the thickness of the absorption layer is about 30nm from pure gold 15, then the uniform transition is carried out to alloy oxide/nitride, and the composition gradient layer is about 170 nm.
The measured reflection spectra before and after annealing are shown in FIG. 5, and the coating reflectivity spectrum before annealing is 21, 550 ℃, 22 after 5h annealing, and 23 after 20h annealing. The spectra before and after annealing are almost unchanged, the reflectivity R is stabilized at about 0.02 and the light absorptivity alpha is stabilized at 0.96 in a solar spectrum band (0.3-2.5 mu m), the reflectivity R reaches 0.92 in an infrared band higher than 2.5 mu m, the thermal radiance epsilon is stabilized at 0.09 and the spectrum absorption selectivity alpha/epsilon is stabilized at 10.7, which shows that the AlCrNbSiTiO high-entropy alloy oxide coating with gradually changed components has good high-temperature stability. The absorptivity α, thermal emissivity ∈ and spectral absorption selectivity α/∈ of the coatings in the second and third examples are shown in table 1, and it can be seen from table 1 that the coatings prepared in the second and third examples have a large spectral absorption potential.
Table 1 shows the absorptance α, the emissivity ε and the spectral absorptance selectivity α/ε of each coating in example two and example three
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method of a solar spectrum absorption coating is characterized by comprising the following steps:
step 1: mounting a target, a substrate and a protective screen between the target and the substrate in sputtering equipment, adjusting the vacuum degree and the temperature of the sputtering equipment to target values, introducing inert gas, and generating plasma at the moment;
step 2: introducing mixed gas flow of oxygen and inert gas or mixed gas flow of nitrogen and inert gas, removing the protective screen, and primarily performing pure gold deposition on the substrate;
and step 3: gradually generating target poisoning on the target along with the progress of deposition, generating a poisoning layer on the surface of the target, continuing the deposition, and depositing a mixture comprising a large amount of alloy and a small amount of alloy oxide/nitride on the substrate;
and 4, step 4: as the deposition continues, the poisoning degree of the target material is deepened, a mixture comprising a small amount of alloy and a large amount of alloy oxide/nitride is deposited on the substrate, the deposition is continued until the target material is completely poisoned, and pure gold oxide/nitride is deposited on the substrate, so that the required solar spectrum absorption layer with a gradual change and gradient structure is obtained.
2. The method for preparing a solar spectrum absorbing coating according to claim 1, wherein the step is continued, and a layer of pure gold oxide and nitride is further deposited on the surface of the prepared gradient coating to be used as an anti-reflection layer, so as to complete the preparation of the solar spectrum absorbing coating containing the absorbing layer and the anti-reflection layer.
3. The method for preparing solar-spectrum absorbing coating according to claim 1, wherein in step 1, the vacuum degree is lower than 10 -3 Pa, temperature between 100 ℃ and 300 ℃.
4. The method for preparing solar spectrum absorbing coating according to claim 1, wherein the flow rate of the mixed gas in step 2 is generally 1.5-5Pa, and the ratio of oxygen to inert gas/nitrogen to inert gas is between 0-1.
5. The method for preparing a solar-spectrum absorbing coating according to claim 1, wherein the target material is a high-entropy alloy.
6. A solar spectrum absorbing coating obtained by the method for preparing a solar spectrum absorbing coating according to any one of claims 1 to 5.
7. The solar spectrum absorbing coating of claim 6, wherein said solar spectrum absorbing coating has a reflectance of not higher than 0.02 and a light absorptivity α of not lower than 0.95 in the band of 0.3-2.5 μm, a thermal radiation ε of not higher than 0.095 in the band of more than 2.5 μm, and a spectral absorption selectivity α/ε of higher than 10.
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