Anti-icing and deicing super-hydrophobic photo-thermal composite material and preparation method thereof

Abstract

The invention relates to the technical field of new materials, in particular to an anti-icing and deicing super-hydrophobic photo-thermal composite material and a preparation method thereof, and the anti-icing and deicing super-hydrophobic photo-thermal composite material is composed of a siloxane modified V4C3 / Cu2S composite material, a low-surface-energy acrylate polymer and a solvent. The siloxane modified V4C3 / Cu2S composite material is prepared from V4C3 / Cu2S modified by a raw material comprising super-hydrophobic silane; the low-surface-energy acrylate polymer is prepared by polymerizing cyclic acrylate, long alkyl chain acrylate and vinyl silicone oil as reaction monomers. The problems that an existing coating is limited in anti-icing performance and poor in durability can be effectively solved.

Description

Technical Field

[0001] The present application relates to the field of new material technology, and more specifically, to an anti-icing and de-icing super-hydrophobic photothermal composite material and a preparation method thereof. Background Art

[0002] Cement-based materials are widely used as building materials worldwide due to their strength, affordability, durability, and plasticity. However, their hydrophilic, porous structure makes them susceptible to water erosion. Especially during the winter months in northern coastal areas, where cement-based materials are exposed to rain and snow for long periods of time, water seeps into their pores and easily freezes, causing volume expansion, which in turn leads to cracking, spalling, and other phenomena that seriously threaten the safety and durability of buildings. However, repairing these buildings is costly, and the raw materials used to produce them also produce additional carbon dioxide, posing a threat to the environment.

[0003] Currently, the main methods for improving the waterproofing and anti-icing properties of cement-based materials include: 1. Adding ultrafine powders such as silica fume, fly ash, and slag to cement-based materials to fill the pores and increase their density; 2. Modifying cement-based materials into superhydrophobicity to reduce surface wettability and improve their impermeability. These methods are specifically categorized as overall superhydrophobicity modification and surface superhydrophobicity modification. Because the addition of ultrafine powders to cement-based materials has limited effectiveness in improving their waterproofing, the hydrophobic admixtures added during overall superhydrophobicity modification pose significant environmental risks.

[0004] Therefore, super-hydrophobic modification of cement-based materials has become a hot topic for improving their waterproof and anti-icing properties due to its simplicity and wide applicability. Among them, the most effective method for super-hydrophobic modification of cement-based materials is to construct a super-hydrophobic coating on the concrete surface.

[0005] However, current research on super-hydrophobic coatings still faces challenges, such as the environmental hazards posed by the fluoropolymers in the materials, the lack of wear resistance, and the limited anti-icing performance and durability of the coatings. Therefore, further research is needed to improve super-hydrophobic coatings. Summary of the Invention

[0006] In view of the problems that the fluorine-containing polymers in the materials of superhydrophobic coatings in the prior art are very harmful to the environment and are not wear-resistant, resulting in limited anti-icing performance and poor durability of the coating; the present application discloses a superhydrophobic photothermal composite material for anti-icing and de-icing and a preparation method thereof. The obtained composite material becomes a green, environmentally friendly, durable superhydrophobic material that can de-icer in all weather conditions.

[0007] In the first aspect, the present application provides an anti-icing and de-icing super-hydrophobic photothermal composite material, which adopts the following technical solution:

[0008] A super-hydrophobic photothermal composite material for anti-icing and de-icing, characterized in that it is composed of raw materials including a siloxane-modified V4C3 / Cu2S composite material, a low-surface-energy acrylate polymer, and a solvent; wherein the mass ratio of the modified V4C3 / Cu2S composite material to the low-surface-energy acrylate polymer is 1:(1.25-3);

[0009] The siloxane-modified V4C3 / Cu2S composite material is prepared by modifying V4C3 / Cu2S with a raw material including superhydrophobic silane. In the V4C3 / Cu2S, Cu2S is distributed in the accordion gaps of the accordion-shaped V4C3 and on the surface of the V4C3.

[0010] The low surface energy acrylate polymer is prepared by polymerization of cyclic acrylate, long alkyl chain acrylate and vinyl silicone oil as reaction monomers.

[0011] By adopting the above technical solution, this application combines an acrylate polymer with excellent properties such as good permeability resistance, strong wear resistance, and strong weather resistance; a silane that forms hydrophobic groups and increases surface roughness upon hydrolysis; and a novel two-dimensional nanomaterial, MXene, which has high conductivity, a large specific surface area, excellent mechanical properties, and good thermal stability. Leveraging the compositional and structural advantages of these three components, the resulting composite material is a green, durable, and all-weather deicing superhydrophobic material.

[0012] Among them, the use of an appropriate amount of siloxane-modified V4C3 / Cu2S composite material and a low-surface-energy acrylate polymer not only makes the material system of the super-hydrophobic material of the present application uniformly dispersed and well-structured, but also does not cause the super-hydrophobicity and adhesive properties of the material to decline, and the various components in the material system can be better compounded. Moreover, the siloxane-modified V4C3 / Cu2S composite material and the low-surface-energy acrylate polymer are used in appropriate amounts, so that the material has good light-heat, electrical conductivity and super-hydrophobicity at the same time.

[0013] Preferably, the mass ratio of the modified V4C3 / Cu2S composite material to the low surface energy acrylate polymer is 1:(1.5-2.14).

[0014] Furthermore, the V4C3 / Cu2S is prepared from copper acetate, multilayer V4C3-MXene material and thiourea in a mass ratio of (0.04-1.6): (0.414): (0.01-0.6).

[0015] Preferably, the V4C3 / Cu2S is prepared from copper acetate, multilayer V4C3-MXene material and thiourea in a mass ratio of (0.05-1.55): (0.414): (0.02-0.6).

[0016] Furthermore, the preparation method of V4C3 / Cu2S comprises the following steps:

[0017] Copper acetate is dissolved in a reaction solvent, wherein the amount ratio (g / ml) of copper acetate to reaction solvent is (0.04-1.6): (35-40), and the mixture is stirred and dissolved to obtain a mixed solution I; then multilayer V4C3-MXene is added to the mixed solution I to obtain a mixed solution II; then thiourea is uniformly dispersed in the mixed solution II, and the solution is maintained at 160-190°C for 16-25 hours to obtain a V4C3 / Cu2S material.

[0018] Preferably, the ratio of cupric acetate to reaction solvent (g / ml) is (0.05-1.55): (35-40). The solution is maintained at 170-180° C. for 19-23 hours to obtain V 4 C 3 / Cu 2 S material.

[0019] By adopting the above technical solution, during the preparation of V4C3 / Cu2S, V4C3-MXene is controlled within a suitable range, avoiding low V4C3-MXene dosages that lead to varying reaction rates and particle agglomeration, and high V4C3-MXene dosages that lead to incomplete reaction, low product purity, and uneven morphology. Excessive amounts of thiourea and copper acetate can lead to incomplete reaction, low product purity, and uneven morphology, while high amounts can cause varying reaction rates. Furthermore, by combining appropriate reaction temperatures and reaction times, the product particle size is uniform, avoiding particle agglomeration and reaction runaway. The use of a reaction solvent helps improve particle dispersibility, ensuring an appropriate reaction rate and a balanced particle size.

[0020] Furthermore, the reaction solvent used in the preparation of V4C3 / Cu2S is at least one of polyethylene glycol 400, polyethylene glycol 200, and polyethylene glycol 300.

[0021] Furthermore, the preparation method of the multilayer V4C3-MXene material comprises the following steps:

[0022] Weigh V4AlC3 powder and slowly add it to an acid solution with a mass fraction of 30%-50% to obtain a precursor solution with a V4AlC3 concentration of (0.03-0.06) g / ml, and then etch and stir at 45-65°C for 24-120h; after stirring, the reactant is cooled to room temperature and centrifuged, and the centrifugal precipitate is centrifuged and washed until the pH value reaches neutral, and then dried in a freeze drying oven to obtain a multilayer V4C3-MXene material.

[0023] Preferably, V4AlC3 powder is weighed and slowly added to an acid solution with a mass fraction of 40% to obtain a precursor solution with a V4AlC3 concentration of 0.045-0.055 g / ml, and then etched and stirred at 50-60°C for 48-96 hours; after stirring, the reactant is cooled to room temperature and centrifuged, and the centrifugal precipitate is centrifuged and washed until the pH value reaches neutral, and then dried in a freeze drying oven for 36h-60h to obtain a multilayer V4C3-MXene material.

[0024] By adopting the above technical solution, a precursor solution of appropriate concentration can avoid over-etching and destruction of the V4AlC3 structure, and can also avoid incomplete etching reaction. In the V4AlC3MAX phase, part of the Al atomic layer is not effectively removed by etching, and no multilayer structure is formed. In addition, the present application etches at 45-65°C, and the temperature will not be too low, thereby making the etching reaction complete. In the V4AlC3MAX phase, part of the Al atomic layer is effectively removed by etching to form a multilayer structure; the temperature will not be too high to avoid excessive reaction and rapid evaporation of the solvent, which is not conducive to the reaction; and the etching stirring time is 24-120h, which will not lead to incomplete etching reaction due to too short time. In the V4AlC3MAX phase, part of the Al atomic layer is not effectively removed by etching and no multilayer structure is formed; nor will it lead to over-etching due to too long time, which will destroy the V4AlC3 structure.

[0025] Furthermore, the acid solution used in the preparation of the multilayer V4C3-MXene material is at least one of hydrofluoric acid, sulfuric acid, and hydrochloric acid.

[0026] By adopting the above technical solution, in the preparation of multilayer V4C3-MXene materials, the acid solution etches the Al atomic layer in the V4AlC3MAX phase to form gaps, thereby forming an accordion-shaped multilayer V4C3TxMXene structure.

[0027] Furthermore, the super-hydrophobic silane is made of an organic solvent, a silane coupling agent, and deionized water, and the silane coupling agent is at least one of phenyltrimethoxysilane, hexadecyltrimethoxysilane, and octadecyltrimethoxysilane.

[0028] Furthermore, the superhydrophobic silane is made of an organic solvent, a silane coupling agent, and deionized water in a mass ratio of 3:(1-5):1. Preferably, the mass ratio of the organic solvent, the silane coupling agent, and the deionized water is 3:(2-4):1.

[0029] Furthermore, the preparation method of the super-hydrophobic silane comprises the following steps:

[0030] An organic solvent, a silane coupling agent, and deionized water are mixed in a mass ratio, and an acid solution is added to adjust the pH to 2-4 (preferably 2-3), and then heated and stirred at 35-65° C. (preferably 45-60° C.) for 2-5 hours (preferably 2.5-4 hours); after the heating and stirring are completed, the reactant is cooled to room temperature, centrifuged, and then centrifuged and washed until the pH value reaches neutral, and then the precipitate is dried in a vacuum drying oven at 50-60° C. to obtain a superhydrophobic silane powder.

[0031] Furthermore, the silane coupling agent is at least one of phenyltrimethoxysilane, hexadecyltrimethoxysilane, and octadecyltrimethoxysilane. Furthermore, the acid solution used in the preparation of the superhydrophobic silane is at least one of formic acid and acetic acid. The particle size of the superhydrophobic silane powder is 8-15 μm.

[0032] By adopting the above technical solution, the organic solvent helps dissolve the silane coupling agent in the hydrolyzed silane coupling agent, achieves uniform dispersion, and controls the hydrolysis rate. The amount of organic solvent controlled in this application is sufficient to ensure that the system has good solubility and stability. At the same time, the amount is not excessive, and the hydrolysis rate is appropriate.

[0033] Deionized water plays the role of providing a hydrolysis medium and removing impurity ions in the hydrolysis of silane coupling agents. The deionized water will not cause incomplete hydrolysis due to too low a dosage. At the same time, the dosage will not be too much to accelerate the hydrolysis and possibly cause problems such as self-polymerization.

[0034] The acid solution plays a role in catalyzing the hydrolysis of the silane coupling agent, controlling the reaction rate, stabilizing the intermediates and improving the uniformity of the reaction. If the pH value is less than 2 after the addition of the acid solution, the hydrolysis will be accelerated and may cause self-polymerization, resulting in decreased solution stability and even possible corrosion of the material surface. If the pH value is greater than 4 after the addition of the acid solution, the hydrolysis rate will be too slow, the self-polymerization will increase, the reaction will be uneven, and ultimately the coverage and performance of the silane coupling agent on the material surface will be affected.

[0035] Furthermore, the mass ratio of the V4C3 / Cu2S to the superhydrophobic silane is 1:(2-10), and the mass ratio of the V4C3 / Cu2S to the superhydrophobic silane is 1:(2.5-9).

[0036] Furthermore, the preparation method of the siloxane-modified V4C3 / Cu2S composite material comprises the following steps:

[0037] V4C3 / Cu2S and superhydrophobic silane are mixed uniformly in an organic solvent, then washed with anhydrous ethanol and dried in a vacuum drying oven at 20-60°C for 36-60 hours to obtain a siloxane-modified V4C3 / Cu2S composite material. The organic solvent can be methanol, ethanol, or isopropanol.

[0038] Furthermore, the raw materials of the low surface energy acrylate polymer include cyclic acrylate, long alkyl chain acrylate, vinyl silicone oil, acetate solvent and initiator, and the mass ratio of the cyclic acrylate, long alkyl chain acrylate, vinyl silicone oil, acetate solvent and initiator is (15-35): (60-160): (15-21): (0.4-0.9).

[0039] Preferably, the mass ratio of long alkyl chain acrylate, vinyl silicone oil, acetate solvent and initiator is (20-30): (75-115): (17-20): (0.5-0.8).

[0040] By adopting the above technical solution, the hydrophobic groups and rigid cyclic structure of cyclic acrylates in the preparation of low-surface-energy acrylic polymers reduce the polymer's surface energy, enhance the material's hydrophobicity, and improve the polymer's mechanical strength while maintaining good flexibility. The long-chain alkyl structure of long-chain acrylates in the preparation of low-surface-energy acrylic polymers reduces the polymer's surface energy, enhancing the material's hydrophobicity, lubricity, and flexibility. Vinyl silicone oil, due to its extremely low surface energy, also reduces the polymer's surface energy, enhancing the material's hydrophobicity, wear resistance, and flexibility. The low-surface-energy acrylic polymer produced by combining these three elements not only exhibits excellent performance on its own but also blends well with the siloxane-modified V4C3 / Cu2S composite material, comprehensively improving material properties. Furthermore, acetate solvents, through their solvent action, adjust viscosity, and improve film-forming properties, ensure smooth polymerization and optimize polymer properties.

[0041] In addition, the appropriate amount of cyclic acrylate, long alkyl chain acrylate and vinyl silicone oil ensures that the polymer polymerization will not be over-polymerized and has an appropriate molecular weight, which effectively improves the mechanical strength, wear resistance, flexibility and stability of the material; and can avoid problems such as excessive polymerization reaction rate, excessively high polymerization molecular weight, increased side reactions, residual monomers, and thus avoid problems such as increased polymer brittleness, decreased flexibility, surface film-forming properties, and decreased hydrophobicity.

[0042] Furthermore, the cyclic acrylate is at least one of cyclohexyl acrylate, isobornyl methacrylate, and cyclohexyl methacrylate; the long alkyl chain acrylate is at least one of tetradecyl acrylate, hexadecyl acrylate, and octadecyl acrylate; and the vinyl silicone oil is at least one of DY-V421 vinyl silicone oil, DY-V401 vinyl silicone oil, and DY-V431 vinyl silicone oil.

[0043] Furthermore, the preparation method of the low surface energy acrylate polymer comprises the following steps:

[0044] Cyclic acrylate, long alkyl chain acrylate and vinyl silicone oil are mixed to obtain a mixed monomer, and then an acetate solvent, the mixed monomer and an initiator are mixed, and heated and stirred at 70-90° C. for 3-5 hours to obtain an acrylic polymer with low surface energy.

[0045] By adopting the above technical solution and appropriate reaction conditions, the reaction can be fully carried out to avoid incomplete polymerization reaction, which will lead to increased brittleness of the polymer, decreased flexibility and decreased hydrophobicity; it can also avoid excessive reaction, which will lead to problems such as deterioration of the mechanical strength, wear resistance, flexibility, stability and increased surface energy of the polymer.

[0046] Furthermore, the raw material solvent in the super-hydrophobic composite material is a mixture of an acetate solvent and an organic alcohol solvent, and the mass ratio of the modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer, the organic alcohol solvent, and the acid ester solvent is 1:(1.25-3):(3-6):(1). The acetate solvent is at least one of methyl acetate, ethyl acetate, propyl acetate, and butyl acetate, and the organic alcohol solvent is at least one of methanol, ethanol, or isopropanol.

[0047] In a second aspect, the present application provides a method for preparing an all-weather anti-icing and de-icing super-hydrophobic composite material, which adopts the following technical solution:

[0048] A method for preparing a super-hydrophobic composite material for all-weather anti-icing and deicing comprises mixing a siloxane-modified V4C3 / Cu2S composite material and a low-surface-energy acrylate polymer to obtain a mixture I, mixing anhydrous ethanol and butyl acetate to obtain a mixture II, and then mixing the mixture I and the mixture II, and ultrasonically mixing them to obtain a super-hydrophobic material capable of all-weather deicing.

[0049] In summary, this application has the following beneficial effects:

[0050] This application combines an acrylate polymer, which exhibits excellent permeability, wear resistance, and weather resistance, with a silane coupling agent, which forms hydrophobic groups and increases surface roughness upon hydrolysis, and a novel two-dimensional nanomaterial, MXene, which exhibits high conductivity, a large specific surface area, excellent mechanical properties, and good thermal stability. Leveraging the compositional and structural advantages of these three components, the resulting composite material is a green, durable, and all-weather deicing superhydrophobic material. BRIEF DESCRIPTION OF THE DRAWINGS

[0051] Figure 1 This is the SEM image of the V4C3-MXene material in Example 3.

[0052] Figure 2This is the SEM image of the V4C3Cu2S material in Example 3. DETAILED DESCRIPTION

[0053] The present application is further described in detail below with reference to the embodiments.

[0054] Example

[0055] This embodiment provides an anti-icing and de-icing super-hydrophobic photothermal composite material and a preparation method thereof, comprising the following steps:

[0056] A. Preparation of low surface energy acrylate polymers;

[0057] First, 15-35 g of cyclic acrylate (at least one of cyclohexyl acrylate, isobornyl methacrylate, and cyclohexyl methacrylate), 60-160 g of long alkyl chain acrylate (at least one of tetradecyl acrylate, hexadecyl acrylate, and octadecyl acrylate), and 15-21 g of vinyl silicone oil (at least one of DY-V421 vinyl silicone oil, DY-V401 vinyl silicone oil, and DY-V431 vinyl silicone oil) are mixed to obtain a mixed monomer. Then, an acetate solvent (methyl acetate, ethyl acetate, propyl acetate, and butyl acetate) having an equal mass as the mixed monomer, the mixed monomer, and 0.4-0.9 g of an initiator (azobisisobutyronitrile, azobisisoheptylonitrile, and dimethyl azobisisobutyrate) are added to a four-necked flask, and the mixture is heated and stirred at 70-90° C. for 3-0.5 hours to obtain an acrylic polymer with low surface energy.

[0058] Preferably, 20g-30g of cyclic acrylate, 75-155g of long alkyl chain acrylate, 17g-20g of vinyl silicone oil, and 0.5g-0.8g of initiator are heated and stirred at 80-87°C for 3.5-4.5 hours to obtain an acrylic polymer with low surface energy.

[0059] B. Preparation of V4C3 / Cu2S;

[0060] Weigh the V4AlC3 powder and slowly add it to a 40% mass fraction of an acid solution (at least one of hydrofluoric acid, sulfuric acid, and hydrochloric acid) to obtain a precursor solution with a concentration of 0.03-0.06 g / ml (preferably 0.045-0.055 g / ml), and then etch and stir at 45-65 ° C (preferably 50-60 ° C) for 48-96 hours. After stirring, the reactant is cooled to room temperature and then centrifuged in a centrifuge. The centrifuged precipitate is then centrifuged and washed with deionized water at a speed of 5000-10000, preferably 6000-8000 rpm, according to a volume ratio of precipitate to washing liquid of 1: (2-5) (preferably 1: (3-4)) until the pH reaches neutral. Subsequently, the multilayer V4C3-MXene material is dried in a freeze dryer for 36h-60h, preferably 48-56h.

[0061] Dissolve 0.04-1.6 g (preferably 0.05-1.55 g) of copper acetate in 30-45 ml (preferably 35-40 ml) of polyethylene glycol (at least one of polyethylene glycol 200, polyethylene glycol 300, or polyethylene glycol 400) under magnetic stirring to obtain mixed solution I. Then, add 0.414 g of vanadium chloride to mixed solution I to obtain mixed solution II. Then, slowly decompose 0.01-0.6 g (preferably 0.01-0.6 g) of thiourea into mixed solution II. Stir continuously for 20-50 minutes, preferably 25-45 minutes. Transfer the solution to a 50 ml Teflon-lined stainless steel autoclave and maintain it at 160-190°C (preferably 170-180°C) for 16-25 hours (preferably 19-23 hours). This yields a vanadium chloride / Cu2S material.

[0062] C. Preparation of siloxane-modified V4C3 / Cu2S composites;

[0063] First, an organic solvent (methanol, ethanol or isopropyl alcohol), a silane coupling agent (at least one of phenyltrimethoxysilane, hexadecyltrimethoxysilane and octadecyltrimethoxysilane) and deionized water are mixed in a mass ratio of 3: (1-5): 1. The preferred mass ratio is 3: (2-4): 1.

[0064] Add to a four-necked flask, add an acid solution (formic acid, acetic acid) to adjust the pH to 2-4, preferably 2-3, and then heat and stir at 35-65 ° C, preferably 45-60 ° C for 2-5 hours (preferably 2.5-4 hours). After heating and stirring, the reactant is cooled to room temperature, then centrifuged using a centrifuge, and then centrifuged in a centrifuge at a speed of 5000-10000, preferably 6000-8000 rpm using an organic solvent (methanol, ethanol or isopropanol water) with a concentration of 80% by weight to wash the centrifuged precipitate until the pH value reaches neutral, and then the precipitate is dried in a vacuum drying oven at 50-60 ° C, preferably 52-58 ° C for 36 hours to 60 hours (preferably 48-56 hours) to obtain a super hydrophobic silane powder.

[0065] V4C3 / Cu2S and superhydrophobic silane powder are mixed in an organic solvent (methanol, ethanol or isopropanol water) in a ratio of 1:(2-10) (preferably 1:2.5-9) and magnetically stirred for 20-50 minutes, preferably 25-45 minutes, and then washed with anhydrous ethanol and dried in a vacuum drying oven at 50-60°C, preferably 52-58°C, for 36h-60h, preferably 48-56h to obtain a siloxane-modified V4C3 / Cu2S composite material.

[0066] D. Preparation of superhydrophobic materials with both passive and active deicing properties;

[0067] The siloxane-modified V4C3 / Cu2S composite material and the acrylate polymer with low surface energy obtained in step A are mixed in a mass ratio of 1:(1.25-3) (preferably 1:(1.5-2.14)) to obtain mixture I. An organic solvent (methanol, ethanol or isopropanol water) and an acetate solvent (methyl acetate, ethyl acetate, propyl acetate or butyl acetate) are mixed in a mass ratio of (3-6):1 to obtain mixture II. Mixture I and mixture II are then mixed and ultrasonicated for 5-20 minutes, preferably 9-15 minutes, to obtain a superhydrophobic material that can both passively and actively de-ice.

[0068] The following is an explanation through specific examples.

[0069] Example 1:

[0070] A. Preparation of low surface energy acrylate polymers;

[0071] First, 15 g of cyclohexyl acrylate, 75 g of tetradecyl acrylate, and 19 g of DY-V421 vinyl silicone oil were mixed to obtain a mixed monomer. Then, methyl acetate, the mixed monomer, and 0.5 g of azobisisobutyronitrile in an amount equal to the mixed monomer were added to a four-necked flask, and the mixture was heated and stirred at 86°C for 4.5 h to obtain an acrylic polymer with low surface energy.

[0072] B. Preparation of V4C3 / Cu2S;

[0073] V4AlC3 powder was weighed and slowly added to 40% hydrofluoric acid to obtain a precursor solution with a concentration of 0.050 g / ml. The solution was then etched and stirred at 55°C for 48 hours. After stirring, the reaction mixture was cooled to room temperature and centrifuged. The precipitate was then washed with deionized water at 8000 rpm in a centrifuge at a 1:3 volume ratio of precipitate to washing solution until the pH reached neutral. The multilayer V4C3-MXene material was then dried in a freeze-dryer for 56 hours.

[0074] Dissolve 0.04g of copper acetate in 40ml of polyethylene glycol 400 under magnetic stirring to obtain mixed solution I. Then, add 0.414g of vanadium chloride to mixed solution I to obtain mixed solution II. Then, slowly decompose 0.114g of thiourea into mixed solution II. Stir continuously for 50 minutes, then transfer the solution to a 50ml Teflon-lined stainless steel autoclave and maintain it at 175°C for 21 hours. This yields the vanadium chloride / Cu2S material.

[0075] C. Preparation of siloxane-modified V4C3 / Cu2S composites;

[0076] First, methanol, phenyltrimethoxysilane, and deionized water were added to a four-necked flask in a mass ratio of 3:1:1. Formic acid was added to adjust the pH to 2, and then heated and stirred at 35°C for 2.5 hours. After heating and stirring, the reactants were cooled to room temperature and then centrifuged. The centrifuged precipitate was then washed with 80% methanol by weight at a volume ratio of 1:2 at 6000 rpm until the pH reached neutral. The precipitate was then dried in a vacuum drying oven at 55°C for 36 hours to obtain a superhydrophobic silane powder.

[0077] V4C3 / Cu2S and superhydrophobic silane powder were mixed in methanol at a ratio of 1:10 and magnetically stirred for 35 minutes, then washed with methanol and dried in a vacuum drying oven at 55°C for 36 hours to obtain a siloxane-modified V4C3 / Cu2S composite material.

[0078] D. Preparation of super-hydrophobic photothermal composite materials for anti-icing and de-icing;

[0079] The siloxane-modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer obtained in step A, methanol and methyl acetate were mixed in a mass ratio of 1:3:3:1 and ultrasonicated for 5 minutes to obtain a superhydrophobic material with both passive and active deicing properties.

[0080] Example 2:

[0081] A. Preparation of low surface energy acrylate polymers;

[0082] First, 35 g of isobornyl methacrylate, 160 g of hexadecyl acrylate, and 21 g of DY-V401 vinyl silicone oil were mixed to obtain a mixed monomer. Then, ethyl acetate, the mixed monomer, and 0.8 g of azobisisoheptonitrile in an amount equal to the mixed monomer were added to a four-necked flask, and the mixture was heated and stirred at 70° C. for 4 hours to obtain an acrylic polymer with low surface energy.

[0083] B. Preparation of V4C3 / Cu2S;

[0084] V4AlC3 powder was weighed and slowly added to 40% sulfuric acid to obtain a precursor solution with a concentration of 0.055 g / ml. The solution was then etched and stirred at 45°C for 120 hours. After stirring, the reaction mixture was cooled to room temperature and centrifuged. The precipitate was then washed with deionized water at 5000 rpm in a centrifuge at a 1:2 volume ratio of precipitate to washing solution until the pH reached neutral. The solution was then dried in a freeze-dryer for 60 hours to obtain a multilayer V4C3-MXene material.

[0085] Dissolve 0.3g of copper acetate in 36ml of polyethylene glycol 200 under magnetic stirring to obtain mixed solution I. Then, add 0.414g of vanadium chloride to mixed solution I to obtain mixed solution II. Then, slowly decompose 0.6g of thiourea into mixed solution II. Stir continuously for 35 minutes, then transfer the solution to a 50ml Teflon-lined stainless steel autoclave and maintain it at 160°C for 23 hours. This yields the vanadium chloride / Cu2S material.

[0086] C. Preparation of siloxane-modified V4C3 / Cu2S composites;

[0087] First, anhydrous ethanol, hexadecyltrimethoxysilane, and deionized water were added to a four-necked flask in a mass ratio of 3:5:1. Acetic acid was added to adjust the pH to 4, and then heated and stirred at 65°C for 3.5 hours. After heating and stirring, the reactants were cooled to room temperature and then centrifuged. The centrifuged precipitate was then washed with 80% ethanol by weight at a volume ratio of 1:4 at 8000 rpm until the pH reached neutral. The precipitate was then dried in a vacuum drying oven at 50°C for 60 hours to obtain a superhydrophobic silane powder.

[0088] V4C3 / Cu2S and superhydrophobic silane powder were mixed in anhydrous ethanol at a ratio of 1 / 4 and magnetically stirred for 45 minutes, then washed with anhydrous ethanol and dried in a vacuum drying oven at 50°C for 60 hours to obtain a siloxane-modified V4C3 / Cu2S composite material.

[0089] D. Preparation of super-hydrophobic photothermal composite materials for anti-icing and de-icing;

[0090] The siloxane-modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer obtained in step A, anhydrous ethanol and ethyl acetate were mixed in a mass ratio of 4:5:6:3 and ultrasonicated for 20 minutes to obtain a superhydrophobic material with both passive and active deicing properties.

[0091] Example 3:

[0092] A. Preparation of low surface energy acrylate polymers;

[0093] First, 25 g of cyclohexyl methacrylate, 155 g of octadecyl acrylate, and 20 g of DY-V401 vinyl silicone oil were mixed to obtain a mixed monomer. Then, butyl acetate, the mixed monomer, and 0.62 g of azobisisobutyronitrile in an amount equal to the mixed monomer were added to a four-necked flask, and the mixture was heated and stirred at 80° C. for 3.5 hours to obtain an acrylic polymer with low surface energy.

[0094] B. Preparation of V4C3 / Cu2S;

[0095] Weigh the V4AlC3 powder and slowly add it to 40% hydrofluoric acid by mass to obtain a precursor solution with a concentration of 0.045g / ml, and then etch and stir at 65°C for 24h. After stirring, the reactants were cooled to room temperature and then centrifuged in a centrifuge. The centrifuged precipitate was then washed with deionized water at a speed of 7000rpm in a centrifuge at a volume ratio of 1:5 between the precipitate and the washing liquid until the pH value reached neutral. Subsequently, the multilayer V4C3-MXene material was obtained by drying in a freeze drying oven for 36h. The structure of the V4C3-MXene material is shown in the figure. Figure 1 shown.

[0096] Dissolve 1.55g of copper acetate in 35ml of polyethylene glycol 400 and dissolve under magnetic stirring to obtain mixed solution I. Then, add 0.414g of V4C3 to mixed solution I to obtain mixed solution II. Subsequently, slowly decompose 0.002g of thiourea into the above mixed solution II, stir continuously for 45min, transfer the solution to a 50ml Teflon-lined stainless steel autoclave, and keep it at 180℃ for 19h. Obtain V4C3 / Cu2S material. The structure of V4C3 / Cu2S material is as follows Figure 2 shown.

[0097] C. Preparation of siloxane-modified V4C3 / Cu2S composites;

[0098] First, anhydrous ethanol, octadecyltrimethoxysilane, and deionized water were added to a four-necked flask in a mass ratio of 3:4:1. Acid solution was added to adjust the pH to 2, and then heated and stirred at 45°C for 2 hours. After heating and stirring, the reactants were cooled to room temperature and then centrifuged. The centrifuged precipitate was then washed with 80% ethanol by weight at a volume ratio of 1:5 at 5000 rpm until the pH reached neutral. The precipitate was then dried in a vacuum drying oven at 60°C for 50 hours to obtain a superhydrophobic silane powder.

[0099] V4C3 / Cu2S and superhydrophobic silane powder were mixed in anhydrous ethanol at a ratio of 1 / 9 and magnetically stirred for 25 min, then washed with anhydrous ethanol and dried in a vacuum drying oven at 60°C for 50 h to obtain a siloxane-modified V4C3 / Cu2S composite material.

[0100] D. Preparation of super-hydrophobic photothermal composite materials for anti-icing and de-icing;

[0101] The siloxane-modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer obtained in step A, anhydrous ethanol and butyl acetate were mixed in a mass ratio of 2:4:5:1 and ultrasonicated for 15 minutes to obtain a superhydrophobic material with both passive and active deicing properties.

[0102] Example 4:

[0103] A. Preparation of low surface energy acrylate polymers;

[0104] First, 20 g of cyclohexyl acrylate, 60 g of tetradecyl acrylate, and 17 g of DY-V431 vinyl silicone oil were mixed to obtain a mixed monomer. Then, propyl acetate, the mixed monomer, and 0.9 g of dimethyl azobisisobutyrate in an amount equal to the mixed monomer were added to a four-necked flask, and the mixture was heated and stirred at 90° C. for 5 hours to obtain an acrylic polymer with low surface energy.

[0105] B. Preparation of V4C3 / Cu2S;

[0106] V4AlC3 powder was weighed and slowly added to 40% hydrochloric acid to obtain a precursor solution with a concentration of 0.06 g / ml. The solution was then etched and stirred at 60°C for 72 hours. After stirring, the reaction mixture was cooled to room temperature and centrifuged. The precipitate was then washed with deionized water at 6000 rpm in a centrifuge with a precipitate-to-wash solution ratio of 1:4 until the pH reached neutral. The multilayer V4C3-MXene material was then dried in a freeze-drying oven for 50 hours.

[0107] Dissolve 1.6g of copper acetate in 45ml of polyethylene glycol 400 under magnetic stirring to obtain mixed solution I. Then, add 0.414g of vanadium chloride to mixed solution I to obtain mixed solution II. Then, slowly decompose 0.6g of thiourea into mixed solution II. Stir continuously for 25 minutes, then transfer the solution to a 50ml Teflon-lined stainless steel autoclave and maintain it at 190°C for 16 hours. This yields the vanadium chloride / Cu2S material.

[0108] C. Preparation of siloxane-modified V4C3 / Cu2S composites;

[0109] First, isopropyl alcohol, hexadecyltrimethoxysilane, and deionized water were added to a four-necked flask in a mass ratio of 3:3:1. Acid solution was added to adjust the pH to 3, and then heated and stirred at 60°C for 5 hours. After heating and stirring, the reactants were cooled to room temperature and then centrifuged. The centrifuged precipitate was then washed with 80% isopropyl alcohol by weight at a ratio of 1:3 between the volume of the precipitate and the washing solution at 7000 rpm until the pH reached neutral. The precipitate was then dried in a vacuum oven at 52°C for 48 hours to obtain a superhydrophobic silane powder.

[0110] V4C3 / Cu2S and superhydrophobic silane powder were mixed in isopropanol in a ratio of 2 / 5 and magnetically stirred for 20 minutes, then washed with isopropanol and dried in a vacuum drying oven at 52°C for 48 hours to obtain a siloxane-modified V4C3 / Cu2S composite material.

[0111] D. Preparation of super-hydrophobic photothermal composite materials for anti-icing and de-icing;

[0112] The siloxane-modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer obtained in step A, isopropyl alcohol and propyl acetate were mixed in a mass ratio of 3:5:4:2 and ultrasonicated for 9 minutes to obtain a superhydrophobic material with both passive and active deicing properties.

[0113] Example 5:

[0114] A. Preparation of low surface energy acrylate polymers;

[0115] First, 30 g of cyclohexyl methacrylate, 116 g of octadecyl acrylate, and 15 g of DY-V431 vinyl silicone oil were mixed to obtain a mixed monomer. Then, propyl acetate, the mixed monomer, and 0.4 g of azobisisobutyronitrile in an amount equal to the mixed monomer were added to a four-necked flask, and the mixture was heated and stirred at 87° C. for 3 hours to obtain an acrylic polymer with low surface energy.

[0116] B. Preparation of V4C3 / Cu2S;

[0117] VA4AlC3 powder was weighed and slowly added to 40% sulfuric acid to obtain a precursor solution with a concentration of 0.03 g / ml. The solution was then etched and stirred at 50°C for 96 hours. After stirring, the reaction mixture was cooled to room temperature and centrifuged. The precipitate was then washed with deionized water at 10,000 rpm in a centrifuge with a precipitate-to-wash solution ratio of 1:4 until the pH reached neutral. The multilayer VA4C3-MXene material was then dried in a freeze-drying oven for 48 hours.

[0118] Dissolve 0.05g of copper acetate in 30ml of polyethylene glycol 400 under magnetic stirring to obtain mixed solution I. Then, add 0.414g of vanadium chloride to mixed solution I to obtain mixed solution II. Then, slowly decompose 0.01g of thiourea into mixed solution II. Stir continuously for 20 hours, then transfer the solution to a 50ml Teflon-lined stainless steel autoclave and maintain it at 170°C for 25 hours. This yields the vanadium chloride / Cu2S material.

[0119] C. Preparation of siloxane-modified V4C3 / Cu2S composites;

[0120] First, anhydrous ethanol, phenyltrimethoxysilane, and deionized water were added to a four-necked flask in a mass ratio of 3:2:1. Acetic acid was added to adjust the pH to 2.5, and then heated and stirred at 55°C for 4 hours. After heating and stirring, the reactants were cooled to room temperature and then centrifuged. The centrifuged precipitate was then washed with 80% ethanol by weight at a ratio of 1:3 in volume at 10,000 rpm until the pH reached neutral. The precipitate was then dried in a vacuum oven at 58°C for 56 hours to obtain a superhydrophobic silane powder.

[0121] V4C3 / Cu2S and superhydrophobic silane powder were mixed in anhydrous ethanol at a ratio of 1 / 2 and magnetically stirred for 50 minutes, then washed with anhydrous ethanol and dried in a vacuum drying oven at 58°C for 56 hours to obtain a siloxane-modified V4C3 / Cu2S composite material.

[0122] D. Preparation of super-hydrophobic photothermal composite materials for anti-icing and de-icing;

[0123] The siloxane-modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer obtained in step A, anhydrous ethanol and propyl acetate were mixed in a mass ratio of 1:5:5:3 and ultrasonicated for 12 minutes to obtain a superhydrophobic material with both passive and active deicing properties.

[0124] Comparative Example

[0125] The difference between Comparative Example 1 and Example 3 is that an equal amount of epoxy resin 6101 (E-44) is used to replace the acrylic resin with low surface energy.

[0126] Comparative Example 2: The difference from Example 3 is that the siloxane-modified V4C3 / Cu2S composite material is not used, and an equal amount of the siloxane-modified V4C3 / Cu2S composite material is used to replace the siloxane-modified V4C3 / Cu2S composite material.

[0127] The difference between Comparative Example 3 and Example 3 is that the siloxane-modified V4C3 / Cu2S composite material, the acrylate polymer with low surface energy obtained in step A, anhydrous ethanol and butyl acetate are mixed in a mass ratio of 1:6:10:1 and ultrasonicated for 15 minutes.

[0128] The difference between Comparative Example 4 and Example 3 is that the preparation process of the low surface energy acrylic ester polymer is as follows: 22.23 g of methyl methacrylate, 44.45 g of ethyl acrylate, and 16.45 g of vinyltrimethoxysilane are mixed to obtain a mixed monomer, and then butyl acetate, the mixed monomer, and 0.638 g of azobisisobutyronitrile in an amount equal to the mixed monomer are added to a four-necked flask, and the mixture is heated and stirred at 80° C. for 3.5 hours to obtain an acrylic polymer with low surface energy.

[0129] Comparative Example 5 differs from Example 3 in that an equal amount of V4C3-MXene material is used in place of V4C3 / Cu2S. The V4C3-MXene material is prepared by slowly adding V4AlC3 powder to 40% hydrofluoric acid to obtain a precursor solution with a concentration of 0.045 g / ml. The solution is then etched and stirred at 65°C for 24 hours. After stirring, the reactants are cooled to room temperature and centrifuged. The centrifuged precipitate is then washed with deionized water at 7000 rpm in a centrifuge at a volume ratio of 1:5 between the precipitate and the washing solution until the pH reaches neutral. The multilayer V4C3-MXene material is then dried in a freeze-drying oven for 36 hours.

[0130] Performance testing

[0131] The composite materials prepared in the examples and comparative examples were tested as follows:

[0132] (1) Freezing time and ice melting time detection, the detection process is as follows:

[0133] The prepared coating material was drop-coated on a concrete block (2×2×2 cm) with a coating thickness of 15 μm. After coating, the concrete block was baked in an oven at 40° C. for 24 h to obtain a test sample.

[0134] The sample was placed on a -15°C refrigeration table, and 10 μL of deionized water was dripped onto the coating. The time from opening the refrigeration table to the time when the droplet became solidified was recorded. This time was the freezing time.

[0135] Drop 10 μL of deionized water onto the sample and place it in a -30°C freezer for 2 hours to completely freeze it. Once frozen, turn on the xenon lamp and adjust the light intensity to 1 sun using a light intensity meter. Then, place the sample under the xenon lamp and record the time from the start of the xenon lamp irradiation to the complete melting of the ice drop. This is the ice melting time.

[0136] (2) Wear resistance test, the testing process is as follows:

[0137] The prepared coating material was drop-coated on a concrete block (2×2×2 cm) with a coating thickness of 15 μm. After coating, the concrete block was baked in an oven at 40° C. for 24 h to obtain a test sample.

[0138] Place the coated side of the sample on 1000-grit sandpaper, place a 1kg weight on the concrete, place a traction rope on the concrete block, and pull the traction rope by hand to move the concrete block on the sandpaper. One cycle is 25cm. Test the contact angle of the sample after 200 cycles.

[0139] The test results are shown in Table 1.

[0140] Table 1 Material performance test table of Examples and Comparative Examples

[0141]

[0142]

[0143] Freezing time and contact angle size are affected by super-hydrophobicity, wherein, generally speaking, the larger the contact angle, the longer the freezing time. The ice melting time is related to the photothermal performance of the photothermal material, and the stronger the photothermal performance, the shorter the ice melting time; as shown by the performance test comparison of the embodiment and the blank group, the composite coating of the present application not only has good anti-icing and deicing performance, but also has excellent wear resistance. Meanwhile, the contact angle of embodiment 1-5 is greater than 150 ° after friction, and still maintains super-hydrophobicity. This is because the present application combines materials such as acrylate polymers, silane coupling agents, and two-dimensional nanomaterials MXene, and uses the advantages of the three compositions and structures to make the resulting composite material become a kind of green, durable, super-hydrophobic material that can de-ice around the clock. Among them, acrylic resin, as the base material of super-hydrophobic silane powder and V4C3 / Cu2S, also possesses certain hydrophobicity and light absorption to heat performance. But it can not reach super-hydrophobicity, and light absorption to heat performance is also extremely limited. The main effect of super-hydrophobic silane powder is to make the coating reach a super-hydrophobic state. As a photothermal material, V4C3 / Cu2S mainly provides photothermal performance.

[0144] Further, analysis of the performance of Comparative Example 1 found that after replacing the acrylic resin with epoxy resin, the various performances of Comparative Example 1 declined to varying degrees. Comparative Example 4 used other acrylate polymers, but in the end, the performance of Comparative Example 4 did not reach the performance advantages of the embodiments of the present application; on the one hand, the acrylate polymer used in this application has the advantages of good anti-permeability, strong wear resistance and strong weather resistance. On the other hand, the use of siloxane-modified V4C3 / Cu2S composite materials and low surface energy acrylate polymers not only makes the material system of the super-hydrophobic material of the present application uniformly dispersed and has a good structure, but also does not cause a decrease in the super-hydrophobicity and adhesion properties of the material, and the various components in the material system can be better compounded.

[0145] Furthermore, analysis of the performance of Comparative Example 2 revealed that the V4C3 / Cu2S composite material was not modified in Comparative Example 2, resulting in significantly decreased deicing and anti-icing performance. This is because silane hydrolysis can form hydrophobic groups and increase surface roughness, improving the performance of the composite material. Without the addition of super-hydrophobic silane powder, the coating loses its super-hydrophobicity, significantly affecting the freezing time and contact angle. Furthermore, analysis of the performance of Comparative Example 3 revealed that, in addition to the use of raw materials, the amount of raw materials used also affects the various properties of the product.

[0146] Furthermore, in Comparative Example 5, where V4C3 / Cu2S is replaced by an equal amount of V4C3-MXene material, the performance also shows a certain degree of decline. This is because the photothermal material in Comparative Example 5 does not generate Cu2S in V4C3, which affects the photothermal performance, so the ice melting performance is greatly affected.

[0147] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A super-hydrophobic photothermal composite material for anti-icing and de-icing, characterized in that: The method comprises raw materials including a siloxane-modified V4C3 / Cu2S composite material, a low-surface-energy acrylate polymer, and a solvent; wherein the mass ratio of the modified V4C3 / Cu2S composite material to the low-surface-energy acrylate polymer is 1:(1.25-3); The siloxane-modified V4C3 / Cu2S composite material is prepared by modifying V4C3 / Cu2S with a raw material including superhydrophobic silane. In the V4C3 / Cu2S, Cu2S is distributed in the accordion gaps of the accordion-shaped V4C3 and on the surface of the V4C3. The low surface energy acrylate polymer is prepared by polymerization of cyclic acrylate, long alkyl chain acrylate and vinyl silicone oil as reaction monomers.

2. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 1, characterized in that: The V4C3 / Cu2S is prepared from copper acetate, multilayer V4C3-MXene material and thiourea in a mass ratio of (0.04-1.6): (0.414): (0.01-0.6).

3. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 2, characterized in that: The preparation method of V4C3 / Cu2S comprises the following steps: Copper acetate is dissolved in a reaction solvent, wherein the amount ratio (g / ml) of copper acetate to reaction solvent is (0.04-1.6): (35-40), and the mixture is stirred and dissolved to obtain a mixed solution I; then multilayer V4C3-MXene is added to the mixed solution I to obtain a mixed solution II; then thiourea is uniformly dispersed in the mixed solution II, and the solution is maintained at 160-190°C for 16-25 hours to obtain a V4C3 / Cu2S material.

4. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 3, characterized in that: The preparation method of the multilayer V4C3-MXene material comprises the following steps: Weigh V4AlC3 powder and slowly add it to an acid solution with a mass fraction of 30%-50% to obtain a precursor solution with a V4AlC3 concentration of (0.03-0.06) g / ml, and then etch and stir at 45-65°C for 24-120h; after stirring, the reactant is cooled to room temperature and centrifuged, and the centrifugal precipitate is centrifuged and washed until the pH value reaches neutral, and then dried in a freeze drying oven to obtain a multilayer V4C3-MXene material.

5. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 1, characterized in that: The mass ratio of the V4C3 / Cu2S to the superhydrophobic silane is 1:(2-10).

6. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 1, characterized in that: The raw materials of the low surface energy acrylate polymer include cyclic acrylate, long alkyl chain acrylate, vinyl silicone oil, acetate solvent and initiator, and the mass ratio of the cyclic acrylate, long alkyl chain acrylate, vinyl silicone oil, acetate solvent and initiator is (15-35): (60-160): (15-21): (0.4-0.9).

7. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 6, characterized in that: The cyclic acrylate is at least one of cyclohexyl acrylate, isobornyl methacrylate, and cyclohexyl methacrylate; the long alkyl chain acrylate is at least one of tetradecyl acrylate, hexadecyl acrylate, and octadecyl acrylate; and the vinyl silicone oil is at least one of DY-V421 vinyl silicone oil, DY-V401 vinyl silicone oil, and DY-V431 vinyl silicone oil.

8. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 1, characterized in that: The preparation method of the low surface energy acrylate polymer comprises the following steps: Cyclic acrylate, long alkyl chain acrylate and vinyl silicone oil are mixed to obtain a mixed monomer, and then an acetate solvent, the mixed monomer and an initiator are mixed, and heated and stirred at 70-90° C. for 3-5 hours to obtain an acrylic polymer with low surface energy.

9. The anti-icing and de-icing super-hydrophobic photothermal composite material according to claim 1, characterized in that: The raw material solvent in the super-hydrophobic composite material is a mixture of an acetate solvent and an organic alcohol solvent, and the mass ratio of the modified V4C3 / Cu2S composite material, the low surface energy acrylate polymer, the ethyl organic alcohol solvent and the acid ester solvent is 1:(1.25-3):(3-6):(1).

10. A method for preparing an all-weather anti-icing and de-icing super-hydrophobic composite material according to any one of claims 1 to 9, characterized in that: A siloxane-modified V4C3 / Cu2S composite material and a low-surface-energy acrylate polymer are mixed to obtain a mixture I, anhydrous ethanol and butyl acetate are mixed to obtain a mixture II, and then the mixture I and the mixture II are mixed and ultrasonically mixed to obtain a superhydrophobic material that can de-ice in all weather conditions.

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