CN109651853B - MoSi stable in high-temperature air2-SiO2Composite photo-thermal coating and preparation method thereof - Google Patents
MoSi stable in high-temperature air2-SiO2Composite photo-thermal coating and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of material preparation, and particularly relates toAnd MoSi stable in high-temperature air2‑SiO2A composite photo-thermal coating and a preparation method thereof. The method adopts silica sol and MoSi2And (3) mixing the powders, forming a black suspension, spin-coating the black suspension on a carrier, drying to obtain a composite layer, and spin-coating the silica sol prepared in the step (2) on the composite layer to form an anti-reflection layer to obtain the composite photo-thermal coating. The coating provided by the invention has the advantages of good high-temperature stability, simple and convenient preparation process, low cost, suitability for large-scale production and the like. And simultaneously has higher solar energy absorptivity. Has important practical value. Meanwhile, the preparation method of the coating has universality and can be used for preparing functional coatings of different filling materials.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to stable MoSi in high-temperature air2-SiO2A composite photo-thermal coating and a preparation method thereof.
Background
The solar photo-thermal absorption coating is a functional coating capable of realizing photo-thermal conversion, and can be used in the fields of solar heat utilization, heat collection type solar power generation and the like. The solar energy has the advantages of cleanness, no pollution, low cost, rich reserves and the like, and has great development potential as a substitute energy of the traditional energy. 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. In recent years, low-temperature photo-thermal technologies, such as solar water heaters, solar houses, and the like, have become popular. In the field of high-temperature photo-thermal application, large-scale photo-thermal-electric conversion equipment such as heat collection type solar power generation is being popularized. Heat collectionThe solar power generation equipment has the advantages of generating alternating current, being convenient for grid connection and the like. However, because of the limited carnot efficiency, such devices must operate at higher temperatures to have higher energy conversion efficiencies. This imposes a necessary requirement on the high temperature stability of its associated components. The photothermal absorption coating is a core component of the heat collection type solar power generation equipment, and the existing photothermal absorption coating has the defects of poor high-temperature stability, complex preparation process, high cost and the like. Theoretically, the focused solar power system achieves the best conversion efficiency (85%) at temperatures of 2480K (2200℃.). However, the working temperature of the photo-thermal absorption coating is generally 750 ℃ at present℃In the following, the demand is far from future, and development is awaited.
Since the idea of solar light-heat-electricity conversion is proposed, research in related fields is being conducted in various countries of the world, and many corresponding achievements have entered the stage of practical use. Such as sorafenac power stations, isaema israel tower solar power stations, etc., in arizona, usa. In recent years, similar solar photo-thermal power generation facilities in China gradually enter the public vision, such as Dunhuang tower type molten salt photo-thermal power stations, the Dunhuang 10 megawatt photo-thermal power stations in the first period are combined with 2017 to generate power, and absolutely clean power can be provided for 3 ten thousand families every year; the second-phase project also enters a debugging stage, the total installed capacity is 100 megawatts, and the annual power generation amount is predicted to be 3.5 hundred million kilowatt hours after the second-phase project is built. 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.
Nowadays, photothermal techniques are already in the low temperature field (<The temperature of 200 ℃ is generally popularized and used, such as a solar water heater, a solar house and the like. The medium-high temperature photo-thermal technology has the defects of poor high-temperature stability, overhigh production cost and the like. The traditional solar photo-thermal absorption coating generally has a complex structure and comprises a plurality of absorption layers, infrared reflection layers, anti-diffusion layers, antireflection layers and the like with different filling ratios. All of these designs require precise component ratios and thickness control, and thus most of the existing coating preparations rely on high costExpensive vacuum deposition equipment such as magnetron sputtering and thermal evaporation. This not only leads to an increase in production cost, but also causes a decrease in production efficiency, which is not favorable for mass production. Meanwhile, due to the fact that the number of layers is large and the structure is complex, the similar solar photo-thermal coating can generate interface element diffusion and internal structure deformation under the high-temperature condition. Such photothermal coatings have been reported to be MoSi2–Si3N4Composite absorber layer of Al/NbMoN/NbMoON/SiO2The maximum working temperature of the multilayer film structure absorbing layer, the self-assembly Al-AlN absorbing layer and the like is mostly lower than 750 ℃, and the multilayer film structure absorbing layer and the self-assembly Al-AlN absorbing layer are limited to be used under the vacuum condition.
Spectrally selective coatings prepared by more economical techniques such as sol-gel methods have also been extensively studied, such as copper-manganese spinel structure photothermal absorbing coatings and Ni-Al2O3Metal ceramic photo-thermal absorption coating and the like. However, the solar photo-thermal absorption coating prepared by the method cannot have high enough thermal stability, and the technical requirements of large-scale heat collection type power generation equipment are difficult to meet.
More recently, black cobalt oxide coatings and Ni-SiO1.5Coatings of this type are reported to be stable in air at 750 ℃ because of a self-terminating oxidation process. However, the best conversion efficiency (85%) is obtained by the focusing solar power generation system at the temperature of 2480K (2200 ℃) so that the thermal stability of the photo-thermal coating has a great improvement space. In addition, the cost is a factor which must be considered in the mass production of the solar energy absorption coating, and how to further improve the thermal stability and reduce the cost is still a problem which is solved firstly.
For example, prior art CN201810545478.0 relates to a MoSi2-SiO2The borosilicate high-temperature-resistant high-emissivity coating comprises the following raw materials in percentage by mass: MoSi2-SiO220-70% of composite powder, 25-80% of borosilicate glass powder and 60-6% of SiB. Firstly, MoO is added2And Si as raw material, preparing MoSi according to a certain proportion2-SiO2The composite powder is used as a high-emissivity phase, the borosilicate glass powder is used as a high-temperature binder, and SiB6 is addedThe agent, polyvinylpyrrolidone PVP as dispersant and ethanol as solvent, to prepare uniform dispersion slurry, and the high temperature resistant high emissivity coating is prepared on the alumina ceramic substrate by adopting a spraying method.
The prior art has the following technical problems: (1) the high temperature stability needs to be improved. (2) The material composition is complex, the production cost is high, the equipment required by production is complex, and the large-scale production is not facilitated. (3) Requiring a vacuum environment and is not suitable for long-term stable use.
Disclosure of Invention
In view of the technical problems in the prior art, the invention provides stable MoSi in high-temperature air2-SiO2The composite photo-thermal coating and the preparation method thereof are realized by the following technical scheme:
MoSi stable in high-temperature air2-SiO2The preparation method of the composite photo-thermal coating comprises the following steps:
(1) carrying out high-energy ball milling reaction on a certain amount of silicon powder and molybdenum powder to prepare MoSi2Powder;
(2) preparing silica sol, namely putting tetraethyl silicate (TEOS) Methyl Triethoxysilane (MTES), ethanol, deionized water and acetic acid into a container for hydrolysis and polycondensation;
(3) mixing the silica sol prepared in the step (2) with MoSi2Mixing the powders, forming a black suspension, spin-coating the black suspension on a carrier, drying to obtain a composite layer, and spin-coating the silica sol prepared in the step (2) on the composite layer to form an anti-reflection layer to obtain MoSi2-SiO2A composite photo-thermal coating.
MoSi selected by the invention2Is a material with better high-temperature stability, and in a high-temperature environment, MoSi2The surface can be combined with oxygen in the air to generate SiO2A barrier layer to prevent further oxidation and to ensure high temperature stability, and if such materials are not used, the coating will not have such good thermal stability. The invention adopts a solvent gel method, and the principle is that liquid precursor sol forms gel after the liquid in the precursor sol is completely volatilized, in this case, silicon dioxide sol is evenly coated on a substrate in a spin modeDrying the liquid to form a film. The scheme has the advantages of simple operation, no dependence on vacuum equipment, low cost and convenience for large-scale production. The antireflection layer increases the sunlight absorption of the coating by the principle of film interference cancellation, and if the antireflection layer is not used, the reflection of the coating is increased and the absorption is reduced.
In a preferred embodiment of the present invention, in the step (1), a high energy ball milling reaction is performed at a molar ratio of Mo to Si of 1 to 3, and the process is performed for 10 hours to obtain MoSi2And (3) powder.
Through a large amount of experimental researches, the method can synthesize MoSi with relatively pure composition2Powder, the high temperature stability of the coating is ensured. In addition, MoSi synthesized by the method2The powder particles are small, so that the powder particles can be dispersed in the silica sol more uniformly.
In the step (2), tetraethyl silicate (TEOS), Methyltriethoxysilane (MTES), ethanol, deionized water and acetic acid, which have the mass of 12.93g, 7.65g, 18.25g, 6.83g and 0.50g, respectively, are added to a 100ml round-bottom flask, and the mixture is magnetically stirred at room temperature for 24 hours, thereby obtaining the transparent silica sol.
A large number of experimental researches find that the silicon dioxide sol is not powder and is liquid, and the sol prepared by the method has proper viscosity and good film forming property. The absence of such a proportion results in an excessively low sol viscosity or poor film-forming properties. Such as excessive ethanol, dilute sol, MoSi2The powder will settle rapidly therein, which is disadvantageous for spin coating. The ethanol consumption is too large, the sol viscosity is too large, the gel is cracked after drying, and a stable coating is not easy to form.
As a preferred technical scheme of the invention, in the step (3), the silica sol and MoSi are mixed2The powder mixture ratio is 1ml of silica sol to 0.1g of MoSi2Powder; in the step (3), the silica sol prepared in the step (2) is spin-coated on the composite layer to form an anti-reflection layer, and the total thickness of the obtained coating is 6.62 mu m.
Through a large amount of experimental researches, the mixture ratio of 1ml of silica sol to 0.1g of MoSi2Powder, and the ratio can obtain the maximum absorption rate of sunlight.
In the step (3), the carrier is made of stainless steel (SUS-304), and is dried in an oven at 80 ℃ for half an hour; this procedure was repeated twice in total. The transparent silica sol was then spin coated on the composite layer to form an antireflective layer, which was dried in an oven at 80 ℃ for half an hour, and this procedure was repeated twice as well.
Through a large amount of experimental researches, thicker coatings can be obtained by repeating twice, the fillers can completely cover the surface of the substrate, the repeated times are unnecessary waste, the coverage of the substrate is incomplete, and the absorption is reduced. Drying at the temperature can completely volatilize the liquid in the sol to form a stable gel coating.
Another object of the present invention is to provide a MoSi stabilized in high temperature air2-SiO2The composite photo-thermal coating is prepared by the preparation method.
The beneficial effects of the invention compared with the prior art comprise:
the coating provided by the invention has the advantages of good high-temperature stability, simple and convenient preparation process, low cost, suitability for large-scale production and the like. And simultaneously has higher solar energy absorptivity. Has important practical value. Meanwhile, the preparation method of the coating has universality and can be used for preparing functional coatings of different filling materials.
Drawings
FIG. 1, MoSi of the invention2-SiO2Schematic diagram of the preparation process of the composite coating.
FIG. 2 MoSi of example 1 of the invention2-SiO2The reflection spectra before and after annealing of the composite coating are shown in FIG. 2a, wherein the reflection spectrum in the wavelength range of 0.2-25 μm is shown in FIG. 2 a. The reflectance spectrum of the coating after annealing at 850 ℃ is shown in FIG. 2b, where the "- -" curve represents the reflectance curve after annealing in air for 10 hours and the "… …" curve represents the reflectance curve after annealing in air for 100 hours.
FIG. 3, the present inventionMoSi of example 12-SiO2Scanning electron microscope images of the surface topography and cross-section of the composite coating, FIG. 3a) MoSi after annealing for 100 hours in air at 850 deg.C2-SiO2The surface appearance of the composite coating, wherein the inner image is a macro-appearance photo, and the outer image is a micro-appearance photo. 3b) Scanning electron micrographs of the cross section of the coating after annealing in air at 850 ℃ for 100 hours. Wherein the upper gray layer is a stainless steel substrate and the middle is MoSi2-SiO2And (3) coating the composite.
FIG. 4 is a graph showing reflection and absorption curves of examples 1, 2 and 3 of the present invention.
FIG. 5, comparative NiSi2-SiO2And MoSi2-SiO2Reflection contrast diagram of the two systems.
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 1
Refer to MoSi shown in FIG. 12-SiO2The preparation process of the composite coating is shown in a schematic diagram,
carrying out high-energy ball milling reaction on a certain amount of molybdenum powder and silicon powder according to the mol ratio of Mo to Si being 1 to 3, and carrying out the process for 10 hours to obtain MoSi2And (3) powder.
The silicon dioxide sol is prepared by adopting a method of tetraethyl silicate (TEOS) hydrolysis and polycondensation. Masses of tetraethyl silicate (TEOS), Methyltriethoxysilane (MTES), ethanol, deionized water and acetic acid, 12.93g, 7.65g, 18.25g, 6.83g and 0.50g, respectively, were charged to 100ml round bottom flasks. Magnetically stirring for 24h at room temperature to obtain transparent silica sol.
Mixing the prepared silica sol and MoSi2Powder mixing (1ml silica sol with 0.1g MoSi)2Powder), formed into a black suspension, was spin-coated on stainless steel (SUS-304), and dried in an oven at 80 ℃ for half an hour. This procedure was repeated twice in total. A transparent silica sol (1ml volume) was then spin coated onto the composite layer to form an antireflective layer, which was dried in an oven at 80 ℃ for half an hour, and this procedure was repeated twice as well.
The reflection spectrum of the obtained coating before annealing in the wavelength range of 0.2-25 μm is shown in FIG. 2 a. The reflectance spectrum of the coating after annealing at 850 ℃ is shown in FIG. 2b, where the "- -" curve represents the reflectance curve after annealing in air for 10 hours and the "… …" curve represents the reflectance curve after annealing in air for 100 hours.
Example 2
The coating obtained with 0.1g MoSi2 powder in combination with 2ml silica sol in exactly the same way as in example 1 has a lower absorption and a reflection spectrum as shown in the "- -" curve of FIG. 4.
Example 3
0.2g MoSi2The powder was mixed with 1ml of silica sol and the coating obtained in exactly the same way as in example 1 had a lower absorption and the reflection spectrum is shown in the curve "… …" in FIG. 4.
Comparative example 1
By using NiSi2-SiO2The procedure of example 1 was repeated. Comparative NiSi2-SiO2And MoSi2-SiO2Two-system experiment shows that MoSi is found2-SiO2The reflectivity of the system in the solar spectrum range is low, the sunlight absorptivity is high, and the specific result is shown in figure 5.
Example 4 Performance testing
Under the condition of only considering normal incidence, the calculation formula of the absorptivity can be simplified as follows:
wherein λ is wavelength, S is total energy (AM 1.5) of standard solar radiation, and S isλIs the standard solar radiation energy of the corresponding wavelength. Is the emissivity of the coating at the corresponding wavelength. According to different wavelength ranges, the ultraviolet-visible-near infrared spectrophotometer and the Fourier transform infrared spectrometer can be used for measurement. Also, considering only normal incidence, the thermal emissivity can be simplified as follows:
wherein I is the total blackbody radiation intensity, IλIs the intensity of the black body radiation at the corresponding wavelength.
Then, the photothermal conversion efficiency of the solar spectrum selective absorption coating is calculated according to the absorptivity alpha and the thermal emissivity, and the photothermal conversion efficiency of the coating is also related to the focusing multiple of sunlight because the conventional sunlight heat collecting equipment does not have single sunlight incidence, but usually obtains larger sunlight incidence amount through optical focusing. Efficiency of photothermal conversion etaPhoto-thermalFollowing the following formula:
wherein σ is the Stefan-Boltzmann constant; t isEnvironment(s)And THigh temperatureAmbient and coating surface temperatures, respectively; etaFocusingIs the optical focusing efficiency, and if the optical loss during focusing is not considered, eta can be consideredFocusingEqual to 1. C is the focusing multiple, and the meaning is the ratio of the radiation area of the sunlight before and after focusing. The photothermal conversion efficiency can be obtained, but as mentioned above, the photothermal conversion efficiency is only an index for measuring the performance of converting sunlight into heat energy, and if the secondary conversion of heat energy by using the carnot heat engine is considered, the overall efficiency of the system follows the following formula:
i.e. the total efficiency is equal to the product of the photothermal conversion efficiency and the carnot efficiency.
The results of the coating absorbance calculations obtained in examples 1, 2 and 3 are shown in table 1:
| examples | Absorption rate (%) |
| 1 | 95.0 |
| 2 | 88.1 |
| 3 | 93.7 |
The results of the calculations of the specific performance parameters of the coating obtained in example 1 are shown in table 2:
TABLE 2 absorptivity, thermal emissivity, photothermal conversion efficiency and overall system efficiency of the coating for different anneals
After annealing the coating in air at 850 ℃ for 10 hours, MoSi2-SiO2Scanning electron microscope images of the surface topography and cross-section of the composite coating, FIG. 3a) MoSi after annealing for 100 hours in air at 850 deg.C2-SiO2The surface appearance of the composite coating, wherein the inner image is a macro-appearance photo, and the outer image is a micro-appearance photo. 3b) Scanning electron micrographs of the cross section of the coating after annealing in air at 850 ℃ for 100 hours. Wherein the upper gray layer is a stainless steel substrate and the middle is MoSi2-SiO2And (3) coating the composite. The coating prepared by the invention has the advantages of good high-temperature stability, higher solar energy absorptivity and the like.
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 (7)
1. MoSi stable in high-temperature air2-SiO2The preparation method of the composite photo-thermal coating comprises the following steps:
(1) carrying out high-energy ball milling reaction on a certain amount of silicon powder and molybdenum powder to prepare MoSi2Powder;
(2) preparing silicon dioxide sol, namely putting tetraethyl silicate (TEOS), Methyltriethoxysilane (MTES), ethanol, deionized water and acetic acid into a container for hydrolysis and polycondensation, respectively adding 12.93g, 7.65g, 18.25g, 6.83g and 0.50g of tetraethyl silicate (TEOS), Methyltriethoxysilane (MTES), ethanol, deionized water and acetic acid into a 100mL round-bottom flask, and magnetically stirring for 24 hours at room temperature to obtain transparent silicon dioxide sol;
(3) mixing the silica sol prepared in the step (2) with MoSi2Mixing the powders, forming a black suspension, spin-coating the black suspension on a carrier, drying to obtain a composite layer, and spin-coating the silica sol prepared in the step (2) on the composite layer to form an anti-reflection layer to obtain MoSi2-SiO2A composite photo-thermal coating.
2. The preparation method according to claim 1, wherein in the step (1), the high energy ball milling reaction is performed at a molar ratio of Mo: Si ═ 1:3, and the process is performed for 10 hours to obtain MoSi2And (3) powder.
3. The method according to claim 1, wherein in the step (3), the silica sol is mixed with MoSi2The powder proportion is 1mL of silica sol and 0.1g of MoSi2The powder, i.e., coating precursor concentration, was 0.1 g/mL.
4. The method according to claim 1, wherein in the step (3), the silica sol prepared in the step (2) is spin-coated on the composite layer to form the anti-reflection layer, and the total thickness of the coating is 6.62 μm.
5. The production method according to claim 1, wherein in the step (3), the support is stainless steel SUS-304, and is dried in an oven at 80 ℃ for half an hour; the steps are repeated for two times, and the composite layer is obtained after drying.
6. The preparation method according to claim 1, wherein in the step (3), the transparent silica sol is spin-coated on the composite layer to form the anti-reflection layer, and the anti-reflection layer is dried in an oven at 80 ℃ for half an hour, and the step is also repeated twice to obtain the composite photothermal coating.
7. MoSi stable in high-temperature air2-SiO2Composite photothermal coating, characterized in that said coating is prepared by the preparation method according to any of the preceding claims 1-6.
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