An adaptive anti-icing composite material and a preparation method and application thereof

Abstract

The application discloses a self-adaptive anti-icing composite material and a preparation method and application thereof, and belongs to the technical field of anti-icing. The ceramic particles and the polymer in the hydrophobic layer of the composite material can increase the roughness of the surface, reduce the surface energy, avoid the accumulation of water on the surface of the material, effectively prevent water from penetrating into the internal structure of the material, and facilitate the entry of electromagnetic waves due to the good impedance matching of the hydrophobic layer. Meanwhile, the porous graphene and the conductive polymer can dissipate electromagnetic waves, achieving the effects of intelligent anti-icing and intelligent stealth. The anti-icing composite material prepared by the application solves the problems of poor adaptability of the surface of the existing wave-absorbing coating, poor adaptability of the anti-icing coating of a stealth aircraft, and the incompatibility of wave-absorbing stealth and icing performance, and has important application prospects in the field of anti-icing.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of anti-icing, and specifically relates to a self-adaptive anti-icing composite material and a preparation method and application thereof. BACKGROUND

[0002] In the field of military aircraft, especially stealth aircraft, the possibility of being detected is reduced by reducing the radar reflection cross section and lowering the infrared radiation. In addition to structural design, it is often necessary to use wave-absorbing materials or stealth coatings to effectively absorb or scatter radar waves to reduce the radar cross section. However, due to the influence of low temperature in winter, icing will occur on the aircraft wings, engine air intakes, and instrument sensor heads, which not only causes certain interference to flight, but also reduces the performance of wave-absorbing coatings. Therefore, the research and innovation of anti-icing materials are crucial to ensure the normal operation of aircraft and flight safety. By continuously optimizing the performance and technology of anti-icing materials, we can better cope with the challenges of adverse weather conditions and ensure the normal flight and task execution efficiency of aircraft. Currently, the development of anti-icing materials mainly includes hydrophobic coatings, anti-freezing coatings, heat-conducting anti-icing materials, and coupled photo-thermal anti-icing technology. The application of these technologies can effectively prolong the time of ice staying on the surface of the aircraft and reduce the adhesion between ice and the surface, thereby improving the anti-icing effect.

[0003] For example, Chen et al. (Pengguang Chen, Shu Tian, Hongshuang Guo et al. An extreme environment-tolerant anti-icing coating[J]. Chemical Engineering Science, 2022, 262, 118010.) prepared an anti-icing coating that can tolerate various extreme environments by incorporating fluorinated amphiphilic copolymer and photo-thermal nanocarbon fibers in the PDMS matrix. This coating can significantly reduce the ice nucleation temperature (<-26℃), increase the icing delay time (~46 times delay), and reduce the ice adhesion strength (~17.7kPa), with excellent anti-icing and energy-saving deicing performance. However, the high temperature generated by the photo-thermal of this coating will weaken the infrared stealth capability.

[0004] Chen et al.(Jichen Chen, Zehui Zhao, Yantong Zhu, et al. Wave-transparent electrothermal composite film for anti-icing / de-icing[J]. Progress in Organic Coatings, 2023, 183, 107751.) prepared a lightweight patterned electrothermal composite film (PEF) using the theory of electromagnetic leakage and frequency selective surfaces, which showed good rapid heating and stability in dynamic ice experiments, and could completely resist ice with only 0.4 W / cm 2 of power density. However, this material needs an external power input, which has the disadvantage of high energy consumption.

[0005] Chinese patent "Intelligent anti-icing material and its preparation method and application" (application number: 201910898261.2, publication number: CN 110591227 A, publication date: 2019.12.20) discloses an intelligent anti-icing material in which nickel-titanium alloy wires are embedded in a hydrophobic resin. When the environmental temperature decreases, the hydrophobic resin will shrink, and the nickel-titanium alloy wires with thermal elastic martensitic phase change characteristics will undergo phase change and expansion, changing the internal expansion force direction of the ice layer, causing micro cracks between the ice layer and the material surface, reducing the adhesion of the ice layer on the material surface, and accelerating the autonomous shedding of the ice layer. The use effect of the material has excellent anti-icing performance without heating. However, repeated shrinkage of the resin and internal martensite may cause a decrease in the adhesion of the coating to the substrate, resulting in peeling of the coating from the substrate.

[0006] Chinese patent "Compatible stealth anti-icing material and its preparation method and application" (application number: 202110913572.9, publication number: CN 113597032, publication date: 2021.11.02) discloses a compatible stealth anti-icing material, which comprises an insulating and heat-insulating layer, a patterned heating layer, an insulating and heat-conducting layer, and a hydrophobic layer arranged in sequence. The synergistic effect of each structure promotes the compatibility of stealth and anti-icing functions. However, its deicing performance depends on the application of an external current, which is not conducive to variable application environments. SUMMARY

[0007] The present application aims to provide a self-adaptive anti-icing composite material and its preparation method and application, to solve the technical problem that the stealth and anti-icing performance of the current stealth aircraft anti-icing coating cannot be compatible, and the environmental adaptability is poor.

[0008] To achieve the above-mentioned purpose, the present application adopts the following technical solutions:

[0009] The application discloses a preparation method of a self-adaptive anti-icing composite material.

[0010] The polymer, ceramic particles, photocrosslinking agent, smoothing agent and defoaming agent are added into a solvent, and are sequentially subjected to stirring, ultraviolet light treatment, filtration and drying treatment to obtain a hydrophobic layer.

[0011] The liquid metal and conductive polymer are added into deionized water, and are sequentially subjected to heating stirring, filtration and drying treatment to obtain a stimulus response layer.

[0012] The stimulus response layer is placed into a water solution containing porous graphene, and is sequentially subjected to oscillation, immersion, filtration and drying treatment to obtain a stimulus response layer decorated with graphene nanosheets.

[0013] The hydrophobic layer is placed in the upper layer, and the stimulus response layer decorated with graphene nanosheets is placed in the lower layer, and then composite hot pressing treatment is performed to obtain the self-adaptive anti-icing composite material.

[0014] Further, when the hydrophobic layer is obtained, the amount of each material is as follows: the polymer is 5-10% by mass, the ceramic particles are 5-10% by mass, the photocrosslinking agent is 1-3% by mass, the smoothing agent is 1-3% by mass, the defoaming agent is 1-5% by mass, and the solvent is 70-75% by mass, and the total amount of the above materials is 100%.

[0015] Further, the polymer is any one of an acrylic polymer, an ether polymer, a fluorocarbon polymer, a polystyrene polymer and a polyvinyl chloride polymer; the ceramic particles are any one of titanium oxide, zinc oxide, cerium oxide and vanadium oxide; the photocrosslinking agent is any one of isopropyl dimethylformamide, acrylate and isocyanate; and the solvent is any two of water, ethanol, methanol and isopropyl alcohol.

[0016] Further, the stirring speed is 100-300 rpm, and the stirring time is 0.5-2 h.

[0017] The ultraviolet light treatment adopts a light source of 300-500 W, and the light irradiation time is 1-3 h.

[0018] The filtration mode is vacuum filtration, the vacuum filtration time is 0.2-1 h, the drying treatment mode is vacuum drying treatment, the vacuum drying treatment temperature is 30-60 DEG C, and the vacuum drying treatment time is 2-8 h.

[0019] Further, the mass ratio of the liquid metal, conductive polymer and deionized water is (0.5-3):(1-3):20, the heating stirring temperature is 40-60 DEG C, and the heating stirring time is 2-8 h.

[0020] The liquid metal is any two of Ga, In and Sn; and the conductive polymer is any one of N(2-hydroxy)propyl 3-trimethyl chitosan chloride, polyaniline, polythiophene and polypyrrole.

[0021] Further, the water solution containing porous graphene is obtained by mixing porous graphene and water; and the concentration of the water solution containing porous graphene is 2-10 mg / L.

[0022] The preparation method of the porous graphene is as follows:

[0023] The graphene, 30% hydrogen peroxide and deionized water are added into a reaction kettle for hydrothermal treatment, and then washed with water, dried at 60 DEG C under vacuum and calcined at 900 DEG C to obtain the porous graphene.

[0024] The volume ratio of the hydrogen peroxide and deionized water is 0.1-2:1-10; and the concentration of the graphene is 2-10 mg / L.

[0025] The hydrothermal treatment is carried out at a temperature of 120-150 DEG C for 1-3 h; the vacuum drying is carried out for 2-4 h; the calcination is carried out for 1-2 h in an atmosphere of any one of nitrogen, argon and hydrogen.

[0026] Further, the oscillation is carried out for 2-6 h; the immersion is carried out by vacuum immersion; the vacuum immersion is carried out for 6-12 h at a vacuum degree of 10 -3 -10 -6 .

[0027] Further, the temperature of the composite hot-pressing treatment is 60-80 DEG C, the time is 0.5-1 h, and the pressure is 5-10 MPa.

[0028] The application further discloses the adaptive anti-icing composite material prepared by the preparation method.

[0029] The application further discloses the application of the adaptive anti-icing composite material, and the adaptive anti-icing composite material is used as a material of an anti-icing coating of a stealth aircraft.

[0030] Compared with the prior art, the application has the following beneficial effects:

[0031] The application discloses a preparation method of a self-adaptive anti-icing composite material, ceramic particles and polymers in a hydrophobic layer of the composite material can increase the roughness of the surface, reduce the surface energy, avoid the accumulation of water on the surface of the material, effectively prevent water from penetrating into the internal structure of the material, and facilitate the entry of electromagnetic waves due to the good impedance matching of the hydrophobic layer; when icing is formed under the influence of freezing rain, the volume expansion of the liquid metal in the stimulation response layer of the composite material is greatly increased under the influence of low temperature, icing pressure and electromagnetic waves, and then the internal conductivity is greatly increased, and then the electric heat conversion is carried out in the porous graphene through the conductive polymer, high heat is generated in the local area, which is helpful to the ablation of the icing into water, and finally the icing is slid off under the assistance of the hydrophobic layer; meanwhile, the porous graphene and the conductive polymer can dissipate electromagnetic waves, and the effects of intelligent anti-icing and intelligent stealth are achieved; the anti-icing composite material prepared by the application solves the problems of poor adaptability of the surface of the existing wave-absorbing coating, and the incompatibility between wave-absorbing stealth and icing performance, and has important application prospect in the field of anti-icing; the preparation method of the application can stably integrate the hydrophobic layer and the stimulation response layer, and obtain a multifunctional composite material with wave-absorbing-electric heating-hydrophobic property, so as to be applicable to the protection of various icing-sensitive equipment and structures. BRIEF DESCRIPTION OF DRAWINGS

[0032] Figure 1 It is a cross-sectional schematic view of the self-adaptive anti-icing composite material of the application.

[0033] Among them: A-hydrophobic layer; B-stimulation response layer; C-ceramic particles; D-liquid metal; E-polymer; F-polymer. DETAILED DESCRIPTION

[0034] In order for those skilled in the art to understand the characteristics and effects of the application, the following is a general description and definition of the terms and phrases mentioned in the specification and claims. Unless otherwise specified, all technical and scientific words used in the text are the usual meanings understood by those skilled in the art of the application, and in case of conflict, the definition in the specification shall prevail.

[0035] Theories or mechanisms described and disclosed herein, whether correct or not, should not limit the scope of the application in any way, i.e., the application can be implemented without being limited by any particular theory or mechanism.

[0036] In this paper, all the characteristics defined in the form of numerical range or percentage range, such as numerical value, quantity, content and concentration, are only for the sake of brevity and convenience. Therefore, the description of numerical range or percentage range should be considered to have covered and specifically disclosed all possible sub-ranges and individual numerical values (including integers and fractions) within the range.

[0037] Herein, unless specifically stated otherwise, "comprise", "comprises", "comprising", "include", "includes", "including", "have", "has", "having" or the like are used in their open-ended, conventional sense, that is they are used to include and refer to the items listed along with additional items, for example, A comprises B means A includes B, but is not limited to B.

[0038] Herein, in order to make the description simple, all possible combinations of the various technical features in the various embodiments or examples are not described. Therefore, as long as there is no contradiction in the combination of the technical features, the various technical features in the various embodiments or examples can be combined arbitrarily, and all possible combinations should be considered as the scope described in the specification.

[0039] The application provides a preparation method of an adaptive anti-icing composite material, comprising the following steps:

[0040] Step 1, preparing a hydrophobic layer;

[0041] 5% to 10% of a polymer, 5% to 10% of ceramic particles, 1% to 3% of a photocrosslinking agent, 1% to 3% of a smoothing agent and 1% to 5% of a defoaming agent are added into 70% to 75% of a solvent, stirring at 100-300 rpm for 0.5-2 h, treating under the irradiation of a 300-500 W ultraviolet lamp for 1-3 h, vacuum filtration for 0.2-1 h and vacuum drying treatment at 30-60 ℃ for 2-8 h, so that the hydrophobic layer is obtained;

[0042] The total amount of the polymer, the ceramic particles, the photocrosslinking agent, the smoothing agent, the defoaming agent and the solvent is 100%; the polymer is any one of an acrylic polymer, an ether polymer, a fluorocarbon polymer, a polystyrene polymer and a polyvinyl chloride polymer; the ceramic particles are any one of titanium oxide, zinc oxide, cerium oxide and vanadium oxide; the photocrosslinking agent is any one of isopropyl dimethylformamide, acrylate and isocyanate; the defoaming agent is any one of polyvinyl alcohol, polysilicone and polysiloxane; the smoothing agent is any one of polysiloxane, synthetic wax and silicone oil; and the solvent is any two of water, ethanol, methanol and isopropyl alcohol.

[0043] Step 2, preparing a stimulus response layer;

[0044] 10-200 μm liquid metal, conductive polymer and deionized water are mixed in a mass ratio of 0.5-3:1-3:20, heated and stirred at 40-60 ℃ for 2-8 h, vacuum filtration for 0.2-1 h and vacuum drying treatment at 30-60 ℃ for 2-8 h, so that the stimulus response layer is obtained; wherein the liquid metal is any two of Ga, In and Sn; and the conductive polymer is any one of N(2-hydroxy)propyl 3 trimethyl chitosan ammonium chloride, polyaniline, polythiophene and polypyrrole.

[0045] Step 3, preparation of porous graphene;

[0046] The graphene with a concentration of 2-10 mg / L, 30% hydrogen peroxide and deionized water are added into a reaction kettle for hydrothermal treatment at 120-150℃ for 1-3h, and then washed with water for 2-4 times, dried at 60℃ for 2-4h under vacuum and calcined at 900℃ for 1-2h to obtain the porous graphene. The volume ratio of hydrogen peroxide and deionized water is 0.1-2:1-10, and the calcination atmosphere is any one of nitrogen, argon and hydrogen.

[0047] Step 4, preparation of a stimulus-responsive layer with graphene nanosheet decoration;

[0048] The obtained stimulus-responsive layer is placed in an aqueous solution containing porous graphene with a concentration of 2-10 mg / L, and then oscillated for 2-6h, vacuum impregnated at 40℃ for 6-12h, vacuum filtered for 0.2-1h and vacuum dried at 30-60℃ for 2-8h to obtain the stimulus-responsive layer with graphene nanosheet decoration, wherein the vacuum degree of vacuum impregnation is 10 -3 -10 -6 .

[0049] Step 5, preparation of self-adaptive anti-icing composite material;

[0050] The hydrophobic layer prepared in step 1 is placed on the upper layer, and the stimulus-responsive layer prepared in step 4 is placed on the lower layer, and then hot-pressed at a pressure of 5-10MPa and a temperature of 60-80℃ for 0.5-1h to obtain the self-adaptive anti-icing composite material.

[0051] Figure 1 is a schematic cross-sectional view of the self-adaptive anti-icing composite material prepared by the present application. As can be seen from the figure, the anti-icing composite material cross-section is composed of a hydrophobic layer A and a stimulus-responsive layer B from top to bottom, wherein a large number of ceramic particles C are embedded in the hydrophobic layer; the stimulus-responsive layer is composed of liquid metal D, polymer E and polymer F.

[0052] The preparation method of the adaptive anti-icing composite material disclosed in the application, by uniformly dispersing ceramic particles in the polymer, through light curing and drying treatment, a hydrophobic layer with high roughness and low surface energy is prepared, the content of ceramic particles and the content of polymer are controlled to obtain a super-hydrophobic layer, which can realize the purposes of preventing water accumulation, water penetration, icing and electromagnetic wave impedance matching on the surface of the material; by adjusting the size of the liquid metal and the content of the conductive polymer and the porous graphene, a stimulation layer with high sensitivity response to pressure, temperature and electromagnetic wave stimulation at low temperature is obtained, which not only realizes high conductivity in the material, but also can perform electric heating conversion to form local high heat in the material, so as to achieve the effect of quickly melting ice into water, and at the same time promote the serious loss of electromagnetic waves inside; the hydrophobic layer and the stimulation layer are combined and treated through hot pressing, the ice formed on the hydrophobic layer is quickly melted into water droplets, the water droplets cannot be maintained on the hydrophobic layer and quickly fall off, and finally the purposes of efficient anti-icing and wave-absorbing stealth are realized.

[0053] At the same time, the ceramic particles and the polymer in the hydrophobic layer of the composite material can increase the roughness of the surface and reduce the surface energy, avoid the accumulation of water on the surface of the material, and effectively prevent water from penetrating into the internal structure of the material, and at the same time, the hydrophobic layer has good impedance matching, which is conducive to the entry of electromagnetic waves; when the ice is formed under the influence of freezing rain, the liquid metal in the stimulation response layer of the composite material is affected by the triple stimulation of low temperature, ice pressure and electromagnetic waves, the internal conductivity is greatly increased, and then the electric heating conversion is carried out through the conductive polymer into the porous graphene, local high heat is generated, which is helpful for the melting of ice into water, and finally the water is assisted to slide on the hydrophobic layer, and at the same time, the porous graphene and the conductive polymer can dissipate electromagnetic waves, so as to achieve the effects of intelligent anti-icing and intelligent stealth. The anti-icing composite material prepared by the application solves the problems of poor adaptability of the surface of the existing wave-absorbing coating, and the incompatibility of stealth and icing performance, and has important application prospect in the field of anti-icing.

[0054] The application will be further described in conjunction with specific examples. It should be understood that these examples are only used to illustrate the application and not to limit the scope of the application. Furthermore, it should be understood that those skilled in the art can make various modifications or changes to the application after reading the content taught by the application, and these equivalent forms also fall within the scope defined by the appended claims of the application.

[0055] In the following examples, conventional instruments and equipment in the art are used. In the following examples, the experimental methods not specified in the specific conditions are usually carried out according to the conventional conditions or according to the conditions recommended by the manufacturer. In the following examples, various raw materials are used, unless otherwise specified, conventional commercially available products are used, and the specifications are conventional specifications in the art. In the specification of the application and the following examples, unless otherwise specified, “%” means weight percent, “parts” means weight parts, and the ratio means weight ratio.

[0056] Example 1

[0057] A method for preparing an adaptive anti-icing composite material, comprising the following steps:

[0058] Step 1, preparing a hydrophobic layer:

[0059] 10% of acrylic polymer, 10% of titanium oxide, 3% of isopropyl dimethylformamide, 1% of polysiloxane and 1% of polyvinyl alcohol were added into 20% of ethanol and 55% of water, stirred at 100 rpm for 0.5 h, treated with 500 W ultraviolet light for 1 h, vacuum filtered for 0.2 h and vacuum dried at 30°C for 2 h, to obtain the hydrophobic layer;

[0060] Step 2, preparing a stimulus-responsive layer:

[0061] 10 μm GaIn (gallium nitride) and N(2-hydroxy)propyl 3 trimethyl chitosan chloride were added into 10 mL of deionized water at a mass ratio of 0.5:1, heated and stirred at 40°C for 2 h, vacuum filtered for 0.2 h and vacuum dried at 30°C for 8 h, to obtain the stimulus-responsive layer;

[0062] Step 3, preparing porous graphene;

[0063] Graphene with a concentration of 2 mg / L, 30% hydrogen peroxide and deionized water were added into a reaction kettle at a volume ratio of 1:2, and hydrothermally treated at 120°C for 3 h, washed with water for 2 times, vacuum dried at 60°C for 2 h and calcined at 900°C in nitrogen for 1 h, to obtain the porous graphene;

[0064] Step 4, preparing a stimulus-responsive layer decorated with graphene nanosheets:

[0065] The stimulus-responsive layer obtained in step 2 was placed in a porous graphene aqueous solution with a concentration of 2 mg / L, oscillated for 2 h, vacuum immersed at 40°C for 6 h, vacuum filtered for 0.2 h and vacuum dried at 30°C for 2 h, to obtain the stimulus-responsive layer decorated with graphene nanosheets, wherein the vacuum degree of vacuum immersion was 10 -3 ;

[0066] Step 5, preparing an adaptive anti-icing composite material:

[0067] The hydrophobic layer prepared in step 1 was placed on the upper layer, and the stimulus-responsive layer prepared in step 4 was placed on the lower layer, and heat-pressed at 60°C for 0.5 h under a pressure of 5 MPa, to obtain the adaptive anti-icing composite material.

[0068] Example 2

[0069] A method for preparing an adaptive anti-icing composite material, comprising the following steps:

[0070] Step 1, preparation of the hydrophobic layer:

[0071] 5% fluorocarbon polymer, 10% zinc oxide, 2% acrylate, 3% synthetic wax and 5% polysilicone were added into 30% propanol and 45% ethanol, stirred at 300 rpm for 1 h, treated with 300 W ultraviolet light for 3 h, vacuum filtered for 1 h and vacuum dried at 60°C for 8 h to obtain the hydrophobic layer;

[0072] Step 2, preparation of the stimulus-responsive layer:

[0073] 200 μm GaSn and polypyrrole were added into 20 mL deionized water at a mass ratio of 1:2, heated and stirred at 60°C for 8 h, vacuum filtered for 1 h and vacuum dried at 60°C for 2 h to obtain the stimulus-responsive layer;

[0074] Step 3, preparation of porous graphene:

[0075] Graphene with a concentration of 10 mg / L, 30% hydrogen peroxide and deionized water were added into a reaction kettle at a volume ratio of 2:10, and hydrothermally treated at 150°C for 1 h, washed with water 4 times, vacuum dried at 60°C for 4 h and calcined at 900°C for 2 h in nitrogen to obtain the porous graphene;

[0076] Step 4, preparation of the stimulus-responsive layer decorated with graphene nanosheets:

[0077] The stimulus-responsive layer obtained in step 2 was placed in a porous graphene aqueous solution with a concentration of 10 mg / L, oscillated for 6 h, vacuum immersed at 40°C for 12 h, vacuum filtered for 1 h and vacuum dried at 60°C for 8 h to obtain the stimulus-responsive layer decorated with graphene nanosheets, wherein the vacuum degree of vacuum immersion was 10 -6 ;

[0078] Step 5, preparation of the self-adaptive anti-icing composite material:

[0079] The hydrophobic layer prepared in step 1 was placed on the upper layer, and the stimulus-responsive layer prepared in step 4 was placed on the lower layer, and the self-adaptive anti-icing composite material was obtained by hot pressing at 80°C for 1 h under a pressure of 10 MPa.

[0080] Example 3

[0081] A method for preparing a self-adaptive anti-icing composite material, comprising the following steps:

[0082] Step 1, preparation of the hydrophobic layer:

[0083] A hydrophobic layer was obtained by adding 8% polyvinyl chloride polymer, 8% vanadium oxide, 2% isocyanate, 2% synthetic wax, and 5% polysiloxane into 45% methanol and 30% ethanol, stirring at 200 rpm for 2 h, treating with 300 W ultraviolet light for 2 h, vacuum filtration for 0.5 h, and vacuum drying at 40°C for 6 h;

[0084] Step 2, preparation of a stimulus-responsive layer:

[0085] A stimulus-responsive layer was obtained by adding 200 μm GaInSn and polyaniline in a mass ratio of 3:1 into 60 mL of deionized water, heating and stirring at 40°C for 6 h, vacuum filtration for 0.5 h, and vacuum drying at 40°C for 6 h;

[0086] Step 3, preparation of porous graphene;

[0087] Porous graphene was obtained by adding graphene with a concentration of 5 mg / L, 30% hydrogen peroxide, and deionized water in a volume ratio of 1:10 into a reaction kettle, hydrothermal treatment at 140°C for 2 h, water washing for 3 times, vacuum drying at 60°C for 3 h, and calcination in nitrogen at 900°C for 1.5 h;

[0088] Step 4, preparation of a stimulus-responsive layer decorated with graphene nanosheets:

[0089] The stimulus-responsive layer obtained in Step 2 was placed in a porous graphene aqueous solution with a concentration of 5 mg / L, oscillated for 4 h, vacuum impregnated at 40°C for 10 h, vacuum filtration for 0.5 h, and vacuum drying at 40°C for 6 h, to obtain a stimulus-responsive layer decorated with graphene nanosheets, wherein the vacuum degree of vacuum impregnation was 10 --5 ;

[0090] Step 5, preparation of an adaptive anti-icing composite material:

[0091] The hydrophobic layer prepared in Step 1 was placed on the upper layer, and the stimulus-responsive layer prepared in Step 4 was placed on the lower layer, and an adaptive anti-icing composite material was obtained by hot pressing at 70°C for 0.7 h under a pressure of 8 MPa.

[0092] Example 4

[0093] A method for preparing an adaptive anti-icing composite material, comprising the following steps:

[0094] Step 1, preparation of a hydrophobic layer:

[0095] A hydrophobic layer was obtained by adding 10% ether polymer, 10% cerium oxide, 2.5% acrylate, 3% silicone oil, and 4.5% polysiloxane into 35% water and 35% methanol, stirring at 250 rpm for 2.5 h, treating with 500 W ultraviolet light for 1.5 h, vacuum filtration for 1 h, and vacuum drying at 50°C for 4 h.

[0096] Step 2, preparation of the stimulus-responsive layer:

[0097] 150 μm InSn and polythiophene were added into 40 mL of deionized water at a mass ratio of 2:3, and were treated by heating stirring at 50°C for 4 h, vacuum filtration for 1 h and vacuum drying at 50°C for 4 h to obtain the stimulus-responsive layer;

[0098] Step 3, preparation of the porous graphene:

[0099] Graphene with a concentration of 8 mg / L, 30% hydrogen peroxide and deionized water were added into a reaction kettle at a volume ratio of 2:5, and were treated by hydrothermal treatment at 130°C for 3 h, water washing for 3 times, vacuum drying at 60°C for 4 h and calcination in nitrogen at 900°C for 1 h to obtain the porous graphene;

[0100] Step 4, preparation of the stimulus-responsive layer with graphene nanosheet decoration:

[0101] The stimulus-responsive layer obtained in Step 2 was placed in a porous graphene aqueous solution with a concentration of 8 mg / L, and was treated by oscillation for 3 h, vacuum impregnation at 40°C for 10 h, vacuum filtration for 0.5 h and vacuum drying at 40°C for 6 h to obtain the stimulus-responsive layer with graphene nanosheet decoration, wherein the vacuum degree of the vacuum impregnation was 10 --4 ;

[0102] Step 5, preparation of the self-adaptive anti-icing composite material:

[0103] The hydrophobic layer prepared in Step 1 was placed on the upper layer, and the stimulus-responsive layer prepared in Step 4 was placed on the lower layer, and was treated by hot pressing at 60°C under a pressure of 6 MPa for 0.8 h to obtain the self-adaptive anti-icing composite material.

[0104] Table 1 is a comparison of the performance of the existing anti-icing coating and the self-adaptive anti-icing composite material prepared in the example, and it can be seen from the table that the self-adaptive anti-icing composite material prepared by the method of the present application can balance the surface anti-icing adaptability, wave absorption stealth and icing performance, and has important application prospects in the field of anti-icing.

[0105] Table 1 is a comparison of the performance of the existing anti-icing coating and the self-adaptive anti-icing composite material prepared in the example, and it can be seen from the table that the self-adaptive anti-icing composite material prepared by the method of the present application can balance the surface anti-icing adaptability, wave absorption stealth and icing performance, and has important application prospects in the field of anti-icing.

[0106]

[0107]

[0108] The above content only illustrates the technical idea of the present application, and cannot limit the protection scope of the present application. Any modification made according to the technical idea of the present application on the basis of the technical solution falls within the protection scope of the claims of the present application.

Claims

1. A method of preparing a self-adapting anti-icing composite material, characterized in that, The method comprises the following steps: The polymer, ceramic particles, photocrosslinking agent, smoothing agent and defoaming agent are added into a solvent, and then are sequentially subjected to stirring, ultraviolet light treatment, filtration and drying treatment to obtain a hydrophobic layer; The liquid metal and conductive polymer are added into deionized water, and then are sequentially subjected to heating stirring, filtration and drying treatment to obtain a stimulus response layer; The stimulus response layer is placed in a porous graphene-containing aqueous solution, and then is sequentially subjected to oscillation, immersion, filtration and drying treatment to obtain a stimulus response layer decorated with graphene nanosheets; The hydrophobic layer is placed on the upper layer, and the stimulus response layer decorated with graphene nanosheets is placed on the lower layer, and then are subjected to composite hot pressing treatment to obtain a self-adaptive anti-icing composite material; In the preparation of the hydrophobic layer, the mass percentage of each material is as follows: polymer 5-10%, ceramic particles 5-10%, photocrosslinking agent 1-3%, smoothing agent 1-3%, defoaming agent 1-5%, solvent 70-75%, and the total of the above materials is 100%. The mass ratio of the liquid metal, conductive polymer and deionized water is (0.5-3):(1-3):20; the heating stirring temperature is 40-60 DEG C, and the time is 2-8 h; The liquid metal is any two of Ga, In and Sn; the conductive polymer is any one of N-(2-hydroxy)propyl-3-trimethyl chitosan ammonium chloride, polyaniline, polythiophene and polypyrrole; The porous graphene-containing aqueous solution is obtained by mixing porous graphene and water; the concentration of the porous graphene-containing aqueous solution is 2-10 mg / L; The preparation method of the porous graphene is as follows: The graphene, 30% hydrogen peroxide and deionized water are added into a reaction kettle for hydrothermal treatment, and then are subjected to water washing, 60 DEG C vacuum drying and 900 DEG C calcination treatment to obtain the porous graphene.

2. The method of claim 1, wherein the self-adapting anti-icing composite material is prepared by the steps of: The polymer is any one of acrylic polymer, ether polymer, fluorocarbon polymer, polystyrene polymer and polyvinyl chloride polymer; the ceramic particles are any one of titanium oxide, zinc oxide, cerium oxide and vanadium oxide; the photocrosslinking agent is any one of isopropyl dimethyl formamide, acrylate and isocyanate; and the solvent is any two of water, ethanol, methanol and isopropyl alcohol.

3. The method of claim 1, wherein the self-adapting anti-icing composite material is prepared by the steps of: The stirring speed is 100-300 rpm, and the time is 0.5-2 h; The ultraviolet light treatment uses a light source of 300-500 W, and the light irradiation time is 1-3 h; The filtration mode is vacuum filtration; the vacuum filtration time is 0.2-1 h; the drying treatment mode is vacuum drying treatment; the vacuum drying treatment temperature is 30-60 DEG C, and the time is 2-8 h.

4. The method of claim 1, wherein the self-adapting anti-icing composite material is prepared by the steps of: The volume ratio of the hydrogen peroxide and deionized water is 0.1-2:1-10; the concentration of the graphene is 2-10 mg / L; The hydrothermal treatment temperature is 120-150 DEG C, and the hydrothermal treatment time is 1-3 h; the vacuum drying time is 2-4 h; the calcination treatment time is 1-2 h; and the calcination treatment atmosphere is any one of nitrogen, argon and hydrogen.

5. The method of claim 1, wherein the self-adapting anti-icing composite material is prepared by the steps of: The oscillation time is 2-6 h; the impregnation mode is vacuum impregnation; the vacuum impregnation time is 6-12 h, the vacuum degree is 10 -3 -10 -6 .

6. The method of claim 1, wherein the self-adapting anti-icing composite material is prepared by the steps of: The temperature of the composite hot-pressing treatment is 60-80 DEG C, the time is 0.5-1 h, and the pressure is 5-10 MPa.

7. A self-adapting anti-icing composite material, characterized in that, The preparation method is prepared by any one of claims 1-6.

8. Use of a self-adapting anti-icing composite material according to claim 7, characterized in that, The adaptive anti-icing composite material is used as a material of an anti-icing coating of a stealth aircraft.

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