CN113480913B - Super-hydrophobic coating with photo-thermal effect, coating and preparation method - Google Patents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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Abstract
The invention relates to a super-hydrophobic coating with a photo-thermal effect, a coating and a preparation method thereof. The preparation method of the coating comprises the following steps: mixing deionized water and ethanol A, and adjusting the pH value to 4-14 to obtain a reaction solvent; adding carbon nanospheres, carbon nanotubes and dopamine hydrochloride into a reaction solvent, and stirring, centrifuging and washing to obtain mixed particles; and uniformly mixing the mixed particles, the ethanol B and the long-chain silane, then adding a resin solution, and continuously and uniformly mixing to obtain the super-hydrophobic coating with the photothermal effect. According to the invention, with the assistance of PDA, the carbon nano material with a strong light absorption effect in a visible-near infrared region is utilized to cooperatively construct a micro-nano rough structure, so that the temperature of the surface of the coating can be rapidly increased to 189 ℃ under the irradiation of simulated sunlight, and the self-repairing of the super-hydrophobic surface can be realized under the action of the sunlight without additionally heating or regulating and controlling the pH value of the coating.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a super-hydrophobic coating with a photo-thermal effect, a coating and a preparation method.
Background
A superhydrophobic surface refers to a surface where the contact angle (WCA) of water with a solid surface is greater than 150 °. Super-hydrophobicity exists widely in nature, such as lotus leaf, rose petal, duckweed, butterfly wing, water strider, mosquito compound eye, etc. In recent years, scientists construct a series of multifunctional artificial super-hydrophobic surfaces by simulating a super-hydrophobic structure generated by natural evolution and by means of a sol-gel method, a spraying method, a template method, an etching method, an electrostatic spinning method, a layer-by-layer self-assembly method and the like. The bionic interface material with excellent performance has attracted extensive attention in the fields of oil-water separation, self-cleaning, frost prevention, corrosion resistance, resistance reduction, pollution prevention and the like.
The artificially constructed hydrophobic surface requires chemical components with proper micro-nano hierarchical structure and low surface energy, and the two are not indispensable. Unfortunately, the micro-nano rough structure with high dependence on the super-wetting property is easy to cause irreversible mechanical damage under the action of external force. In addition, under severe environments such as corrosive media (acids, alkalis and salts), strong ultraviolet irradiation and high temperature, the low surface energy substance modified by the super-hydrophobic surface is often damaged or contaminated due to adsorbed impurities. These all result in a reduction in the inherent hydrophobic properties of the coating. Therefore, the durability and stability problems of the superhydrophobic coating under different environments become one of the limitations of its large-scale application.
Over the last few years, researchers have conducted extensive research into the construction of wear resistant, stable super-wetting surfaces from different perspectives. One is to extend the lifetime of the superhydrophobic material by preparing free standing samples. The second is the use of strong binders such as epoxy, polydimethylsiloxane and aluminum phosphate to improve the adhesion of the coating to the substrate. Thirdly, the coating is endowed with self-repairing capability through external stimulation such as heating, pH and the like, and the long-term durability of the coating is improved. However, most self-repairing processes of self-repairing super-hydrophobic coatings require heating or pH regulation, so that the problems of high energy consumption and inconvenient operation exist.
Disclosure of Invention
In view of the above, there is a need to provide a superhydrophobic coating with a photo-thermal effect, a coating and a preparation method thereof, so as to solve the technical problems of high energy consumption and inconvenient operation in the self-repairing process of the self-repairing superhydrophobic coating in the prior art.
The first aspect of the invention provides a preparation method of a super-hydrophobic coating with a photo-thermal effect, which comprises the following steps:
mixing deionized water and ethanol A, and adjusting the pH value to 4-14 to obtain a reaction solvent;
adding carbon nanospheres, carbon nanotubes and dopamine hydrochloride into the reaction solvent, and stirring, centrifuging and washing to obtain mixed particles;
and uniformly mixing the mixed particles, the ethanol B and the long-chain silane, then adding a resin solution, and continuously and uniformly mixing to obtain the super-hydrophobic coating with the photo-thermal effect.
The second aspect of the invention provides a super-hydrophobic coating with a photo-thermal effect, which is obtained by the preparation method of the super-hydrophobic coating with the photo-thermal effect provided by the first aspect of the invention.
A third aspect of the present invention provides a self-healing superhydrophobic coating having a photo-thermal effect, which is formed by coating the superhydrophobic coating having a photo-thermal effect obtained by the first aspect of the present invention on a substrate and curing.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a layer of Polydopamine (PDA) is modified on the surface of a carbon nano material by utilizing dopamine hydrochloride spontaneous oxidation polymerization, a micro-nano rough structure is cooperatively constructed by utilizing the carbon nano material with a strong light absorption effect in a visible-near infrared region with the assistance of the PDA, the hole structure is not only necessary for super-hydrophobicity, but also can obviously improve the photo-thermal conversion effect of the coating, the temperature of the surface of the coating can be rapidly increased to 189 ℃ under the irradiation of simulated sunlight, the pH value of the coating does not need to be additionally heated or regulated, and the self-repairing of the super-hydrophobic surface can be realized under the action of the sunlight; the self-repairing super-hydrophobic coating with the photo-thermal effect has the advantages of simplicity, low cost and environmental protection, and has good application prospects in the fields of self-repairing, ice-resistant defrosting, water collection, crude oil leakage and the like.
Drawings
FIGS. 1(a) - (b) are Scanning Electron Microscope (SEM) images of the superhydrophobic coatings prepared in example 3 and comparative example 1, respectively;
FIG. 2 is a photograph of the contact angle and sliding angle of a water drop of the superhydrophobic coating prepared in example 3;
in fig. 3, (a) to (d) are respectively the images of the infrared imager of the super-hydrophobic coatings prepared in example 3 and comparative examples 1 to 3 at the highest temperature under the simulated solar irradiation (I ═ 20A);
FIG. 4 is a schematic representation of the super-hydrophobic and super-hydrophilic transition process for the coating prepared in example 3;
FIG. 5 is a graph of the cyclic change in water contact angle during the superhydrophobic and superhydrophilic transition for the coatings prepared in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The first aspect of the invention provides a preparation method of a super-hydrophobic coating with a photo-thermal effect, which comprises the following steps:
s1, mixing deionized water and ethanol A, and adjusting the pH value to 4-14 to obtain a reaction solvent;
s2, adding the carbon nanospheres, the carbon nanotubes and dopamine hydrochloride into the reaction solvent, and stirring, centrifuging and washing to obtain mixed particles;
s3, uniformly mixing the mixed particles, ethanol B and long-chain silane, then adding a resin solution, and continuously uniformly mixing to obtain the super-hydrophobic coating with the photo-thermal effect.
In step S1 of the present invention, the mass ratio of deionized water to ethanol a is 1: (0.01-10). According to the invention, deionized water and ethanol A are mixed and pH is adjusted to be used as a reaction solvent, so that the dispersion effects of the carbon nanospheres, the carbon nanotubes and dopamine hydrochloride can be improved.
In some embodiments of the invention, the mass ratio of deionized water to ethanol a is 1: 1.
In some preferred embodiments of the present invention, the reaction solvent has a pH of 8 to 10, and more preferably 8.5.
In some embodiments of the invention, the pH is adjusted by adding a lye. Further, the alkali liquor is at least one of ammonia water or NaOH solution.
In step S2, the diameter of the carbon nanospheres is 100-500 nm; the carbon nanotube has a length of 8 to 15 μm, an inner diameter of 3 to 5nm, and an outer diameter of 8 to 15 nm.
In step S2 of the present invention, the ratio of the amount of the reaction solvent to the amount of the carbon nanospheres, the carbon nanotubes, and dopamine hydrochloride is 1 mL: (1-15) mg: (0.1-10) mg: (1-15) mg.
In some preferred embodiments of the present invention, the ratio of the reaction solvent to the nano carbon spheres, the carbon nanotubes and the dopamine hydrochloride is 1 mL: (1-3) mg: (0.5-10) mg: (1-3) mg.
In some preferred embodiments of the invention, the mass ratio of the carbon nanospheres to the carbon nanotubes is 1 (0.5-4), and further 1: 2; the mass ratio of the total mass of the carbon nanospheres and the carbon nanotubes to the dopamine hydrochloride is 3: 1. Under the condition of the mass ratio, the obtained super-hydrophobic coating has optimal super-hydrophobic performance.
In step S2, the carbon nanospheres, the carbon nanotubes, and dopamine hydrochloride are added to the reaction solvent, followed by stirring for 20-60 hours.
In step S3 of the present invention, the ratio of the total mass of the carbon nanospheres and carbon nanotubes in step S2 to the amount of ethanol B is (1-15) mg: 1mL, further (3-10) mg: 1 mL.
In step S3, the long-chain silane is one or more of dodecyl trimethoxy silane, dodecyl triethoxy silane, dodecyl methyl dimethoxy silane, hexadecyl trimethoxy silane and octadecyl trimethoxy silane; the dosage ratio of the long-chain silane to the ethanol B is 10-100 mu L: 1mL, further 15 μ L: 1 mL.
In step S3, the mixed particles, ethanol B and long-chain silane are uniformly mixed by stirring for 2-10 h.
In step S3 of the present invention, the resin used in the resin solution is one or more of epoxy resin, fluorocarbon resin, phenolic resin, polyester resin, and polyamide resin; the concentration of the resin solution is 10-100 mg/mL, and further 60 mg/mL; the dosage ratio of the resin solution to the ethanol B is 1 (2-10), and further 1: 4. By adding the resin solution in the present invention, the mechanical properties and adhesion properties to the substrate of the resulting coating can be improved. The addition of the resin needs to be strictly controlled, if the addition of the resin is too much, the hydrophobicity of the coating is reduced, and the super-hydrophobic coating cannot be obtained, and if the addition of the resin is too little, the mechanical property of the coating is not obviously improved.
In step S3 of the present invention, the mixed solution of the mixed particles, ethanol B, and long-chain silane and the resin solution are continuously and uniformly mixed by means of ultrasound. Furthermore, the time of ultrasonic treatment is 20-40 min, and further 30 min.
The second aspect of the invention provides a super-hydrophobic coating with a photo-thermal effect, which is obtained by the preparation method of the super-hydrophobic coating with the photo-thermal effect provided by the first aspect of the invention.
A third aspect of the present invention provides a self-healing superhydrophobic coating having a photo-thermal effect, which is formed by coating the superhydrophobic coating having a photo-thermal effect obtained by the first aspect of the present invention on a substrate and curing.
In the present invention, the coating manner is at least one of spray coating, dip coating or spin coating.
In the invention, the substrate is one or more of glass sheet, aluminum alloy sheet, copper sheet, plastic, wood block, fabric, sponge or paper.
In the invention, the curing temperature is 40-120 ℃, and the curing time is 2-4 h.
The self-repairing super-hydrophobic coating with a unique micro-nano structure is obtained through the synergistic effect of the carbon nanospheres, the carbon nanotubes and the dopamine hydrochloride; the self-repairing super-hydrophobic coating has a strong light absorption effect in a visible-near infrared region, so that the surface temperature of the coating can be quickly increased to 189 ℃ under simulated sunlight (I ═ 20A) radiation, and the thermal migration of a silane long chain can be realized; when the coating is subjected to O2When the super-hydrophobic performance is lost due to chemical attacks such as plasma etching or salt spray, the super-hydrophobic performance can be quickly recovered through solar irradiation, the service life of the coating in various severe environments is effectively prolonged, extra heating or pH (potential of hydrogen) regulation of the coating is not needed, and self-repairing of the super-hydrophobic surface can be realized under the action of sunlight; compared with the common photo-thermal coating, the water repellency and self-cleaning capability of the coating can keep the surface of the substrate dry and tidy, and the shielding and scattering of water or pollutants to sunlight are avoided, so that the coating can keep higher photo-thermal efficiency for a long time and has good energy-saving effect.
The contact angle test analysis of the invention adopts a Kruss DSA100 (Germany) drop shape analyzer; scanning Electron Microscope (SEM) test adopts Zeiss Ultra Plus (German Zeiss) field emission scanning electron microscope; a xenon lamp current-stabilized power supply (PLS-SXE300) is adopted as a light source of the simulated sunlight; coating temperature testing was provided by a FLIR infrared imager (usa); using O2And carrying out super-hydrophilic treatment on the coating by using a plasma cleaning machine.
In the following examples and comparative examples of the present invention, some of the raw materials are summarized as follows:
the resin solution was obtained by dispersing 0.3g of a mixture made of E51 epoxy resin and 0.09g W93 curing agent (modified amine) in a mass ratio of 10:3 in 5mL of ethanol;
the diameter of the nano carbon sphere is about 385 nm;
the carbon nanotube has a length of 8 to 15 μm, an inner diameter of 3 to 5nm, and an outer diameter of 8 to 15 nm.
Example 1
A preparation method of a self-repairing super-hydrophobic coating with a photo-thermal effect comprises the following steps:
(1) dissolving 10mL of ethanol in 10mL of deionized water at room temperature, and adding 2 wt% of NaOH solution to adjust the pH value to 8.5 to obtain a reaction solvent;
(2) sequentially adding 40mg of carbon nanospheres, 20mg of carbon nanotubes and 40mg of dopamine hydrochloride into the reaction solvent under stirring, continuously stirring for 24 hours, and centrifuging and washing to obtain mixed particles;
(3) dispersing the mixed particles into 20mL of ethanol, adding 300 mu L of dodecyl trimethoxy silane, stirring for 4h, then adding 5mL of resin solution (the concentration is 60mg/mL), and performing ultrasonic treatment to uniformly mix the resin solution to obtain the super-hydrophobic coating with the photothermal effect;
(4) and (3) coating the super-hydrophobic coating with the photo-thermal effect on a glass substrate in a spraying manner, and drying in an oven at 80 ℃ for 3h to obtain the self-repairing super-hydrophobic coating with the photo-thermal effect.
The coating prepared in this example was measured to have a water contact angle of 156.1 ° and a sliding angle of 10.9 °, and to have superhydrophobic properties.
Example 2
A preparation method of a self-repairing super-hydrophobic coating with a photo-thermal effect comprises the following steps:
(1) dissolving 10mL of ethanol in 10mL of deionized water at room temperature, and adding 2 wt% of NaOH solution to adjust the pH value to 8.5 to obtain a reaction solvent;
(2) sequentially adding 40mg of carbon nanospheres, 40mg of carbon nanotubes and 40mg of dopamine hydrochloride into the reaction solvent under stirring, continuously stirring for 24 hours, and centrifuging and washing to obtain mixed particles;
(3) dispersing the mixed particles into 20mL of ethanol, adding 300 mu L of dodecyl trimethoxy silane, stirring for 4h, then adding 5mL of resin solution (the concentration is 60mg/mL), and performing ultrasonic treatment to uniformly mix the resin solution and the resin solution to obtain the super-hydrophobic coating with the photothermal effect;
(4) and (3) coating the super-hydrophobic coating with the photo-thermal effect on a glass substrate in a spraying manner, and drying in an oven at 80 ℃ for 3h to obtain the self-repairing super-hydrophobic coating with the photo-thermal effect.
The coating prepared in this example was found to have a water contact angle of 159.8 ° and a sliding angle of 7.7 °, with superhydrophobic properties.
Example 3
A preparation method of a self-repairing super-hydrophobic coating with a photo-thermal effect comprises the following steps:
(1) dissolving 10mL of ethanol in 10mL of deionized water at room temperature, and adding 2 wt% of NaOH solution to adjust the pH value to 8.5 to obtain a reaction solvent;
(2) sequentially adding 40mg of carbon nanospheres, 80mg of carbon nanotubes and 40mg of dopamine hydrochloride into the reaction solvent under stirring, continuously stirring for 24 hours, and centrifuging and washing to obtain mixed particles;
(3) dispersing the mixed particles into 20mL of ethanol, adding 300 mu L of dodecyl trimethoxy silane, stirring for 4h, then adding 5mL of resin solution (the concentration is 60mg/mL), and performing ultrasonic treatment to uniformly mix the resin solution and the resin solution to obtain the super-hydrophobic coating with the photothermal effect;
(4) and (3) coating the super-hydrophobic coating with the photo-thermal effect on a glass substrate in a spraying manner, and drying in an oven at 80 ℃ for 3h to obtain the self-repairing super-hydrophobic coating with the photo-thermal effect.
Referring to fig. 1(a) and fig. 2, under the action of dopamine hydrochloride, the carbon nanospheres and the carbon nanotubes cooperatively construct a micro-nano rough structure, and the obtained coating has a surface roughness Sa of 15.6, a water contact angle of 160.7 °, and a sliding angle of 4.0 °.
Referring to fig. 3(a), the surface temperature of the coating prepared in this example can be rapidly increased to 189 ℃ under the irradiation of the simulated solar light.
Example 4
A preparation method of a self-repairing super-hydrophobic coating with a photo-thermal effect comprises the following steps:
(1) dissolving 10mL of ethanol in 10mL of deionized water at room temperature, and adding 2 wt% of NaOH solution to adjust the pH value to 8.5 to obtain a reaction solvent;
(2) sequentially adding 40mg of carbon nanospheres, 160mg of carbon nanotubes and 40mg of dopamine hydrochloride into the reaction solvent under stirring, continuously stirring for 24 hours, and centrifuging and washing to obtain mixed particles;
(3) dispersing the mixed particles into 20mL of ethanol, adding 300 mu L of dodecyl trimethoxy silane, stirring for 4h, then adding 5mL of resin solution (the concentration is 60mg/mL), and performing ultrasonic treatment to uniformly mix the resin solution and the resin solution to obtain the super-hydrophobic coating with the photothermal effect;
(4) and (3) coating the super-hydrophobic coating with the photo-thermal effect on a glass substrate in a spraying manner, and drying in an oven at the temperature of 80 ℃ for 3h to obtain the super-hydrophobic coating with the photo-thermal effect.
The coating prepared in this example was found to have a water contact angle of 153.7 ° and a sliding angle of 3.6 ° and to have superhydrophobic properties.
Comparative example 1
The only difference compared to example 3 is that step (2) of comparative example 1 is: and sequentially adding 40mg of nano carbon spheres and 80mg of carbon nano tubes into the reaction solvent under the stirring state, continuously stirring for 24 hours, centrifuging and washing to obtain mixed particles.
Referring to fig. 1(b), the coating obtained in comparative example 1 has a relatively flat structure, a surface roughness Sa of 12.8, a water contact angle of 153.4 °, and a sliding angle of 11.0 °; referring to fig. 3(b), the temperature of the surface of the resulting coating can only rise to 167 ℃ under simulated solar radiation.
Comparative example 2
The only difference compared to example 3 is that step (2) of comparative example 2 is: and sequentially adding 120mg of carbon nanospheres and 40mg of dopamine hydrochloride into the reaction solvent under stirring, continuously stirring for 24 hours, centrifuging and washing to obtain mixed particles.
The coating prepared in this comparative example was measured to have a water contact angle of 152.1 ° and a sliding angle of 25.4 °. Referring to fig. 3(c), the temperature of the surface of the resulting coating can be raised to 141 ℃ under simulated solar radiation.
Comparative example 3
The only difference compared to example 3 is that step (2) of comparative example 3 is: and sequentially adding 120mg of carbon nano tube and 40mg of dopamine hydrochloride into the reaction solvent under the stirring state, continuously stirring for 24 hours, centrifuging and washing to obtain mixed particles.
The coating prepared in this comparative example was measured to have a water contact angle of 155.9 ° and a sliding angle of 6.9 °. Referring to fig. 3(d), the temperature of the resulting coating surface can be raised to 176 ℃ under simulated solar radiation.
According to the results of the embodiments 1-4 and the comparative examples 2-3, the nano carbon spheres and the carbon nanotubes are added to cooperatively construct the micro-nano coarse structure, so that the hydrophobic property of the coating can be obviously improved; the mass ratio of the carbon nanospheres to the carbon nanotubes has a great influence on the hydrophobicity of the obtained coating, and when the mass ratio of the carbon nanospheres to the carbon nanotubes is 1:2, the obtained coating has the best hydrophobic property.
Meanwhile, as can be seen from the results of example 3 and comparative example 1, the addition of dopamine hydrochloride is more favorable for forming a rough structure, and the hydrophobic property and the photothermal conversion effect are improved.
Referring to FIGS. 4-5, O is used2After the plasma cleaning machine carries out hydrophilic treatment on the coating, the obtained coating is converted from super-hydrophobic to super-hydrophilic; after the super-hydrophilic surface is subjected to solar irradiation treatment for 3-5 min, the super-hydrophobic surface is restored to be a super-hydrophobic surface, and the super-hydrophobic self-healing coating can realize the super-hydrophobic self-healing under the solar irradiation condition without additional heating or pH regulation.
While the invention has been described with reference to specific preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the following claims.
Claims (8)
1. A preparation method of a super-hydrophobic coating with a photo-thermal effect is characterized by comprising the following steps:
mixing deionized water and ethanol A, and adjusting the pH value to 4-14 to obtain a reaction solvent;
adding carbon nanospheres, carbon nanotubes and dopamine hydrochloride into the reaction solvent, and stirring, centrifuging and washing to obtain mixed particles; the dosage ratio of the reaction solvent to the carbon nanospheres, the carbon nanotubes and the dopamine hydrochloride is 1 mL: (1-15) mg: (0.1-10) mg: (1-15) mg; the mass ratio of the carbon nanospheres to the carbon nanotubes is 1 (0.5-4);
and uniformly mixing the mixed particles, the ethanol B and the long-chain silane, then adding a resin solution, and continuously and uniformly mixing to obtain the super-hydrophobic coating with the photo-thermal effect.
2. The method for preparing the superhydrophobic coating with the photothermal effect according to claim 1, wherein the mass ratio of the deionized water to the ethanol a is 1: (0.01-10).
3. The preparation method of the superhydrophobic coating with the photothermal effect according to claim 1, wherein the ratio of the total mass of the carbon nanospheres and the carbon nanotubes to the amount of ethanol B is (1-15) mg: 1 mL.
4. The preparation method of the superhydrophobic coating with the photothermal effect according to claim 1, wherein the dosage ratio of the long-chain silane to the ethanol B is 10-100 μ L: 1 mL.
5. The method for preparing the superhydrophobic coating having the photothermal effect according to claim 1, wherein the resin used in the resin solution is one or more of epoxy resin, fluorocarbon resin, phenolic resin, polyester resin, and polyamide resin.
6. The preparation method of the superhydrophobic coating with the photothermal effect is characterized in that the concentration of the resin solution is 10-100 mg/mL, and the dosage ratio of the resin solution to the ethanol B is 1 (2-10).
7. The super-hydrophobic coating with the photo-thermal effect is characterized by being obtained by the preparation method of the super-hydrophobic coating with the photo-thermal effect according to any one of claims 1 to 6.
8. The self-repairing super-hydrophobic coating with the photo-thermal effect is formed by coating the super-hydrophobic coating with the photo-thermal effect obtained by the preparation method of the super-hydrophobic coating with the photo-thermal effect of any one of claims 1 to 6 on a substrate and curing.
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CN114605855B (en) * | 2022-03-20 | 2022-11-08 | 南昌大学 | Preparation method of super-hydrophobic coating with anti-icing/deicing function |
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