Anti-icing composite coating with transition layer structure as well as preparation method and application of anti-icing composite coating

Abstract

The invention discloses an anti-icing composite coating with a transition layer structure as well as a preparation method and application of the anti-icing composite coating. Belongs to the technical field of wind power generation protective coatings. An anti-icing composite coating with a transition layer structure comprises a substrate, and a transition layer and a top layer are introduced on the substrate; the substrate is made of a blade-shaped metal or alloy material; the transition layer is an epoxy metal primer coating; and the top layer is an epoxy organic silicon hybrid resin coating. A transition layer mechanism is introduced into the obtained coating, under the condition that the hydrophobic / anti-icing capacity of the coating is not affected, the situation that the elastic modulus and the thermal expansion coefficient of different coatings are not matched is reduced, meanwhile, the air hole or hole defect in the coating preparation process is reduced, the coating has high mechanical durability and abrasion resistance, and the service life of the coating is prolonged. The high-speed water washing resistance is obviously improved.

Description

Technical Field

[0001] The present invention relates to an anti-icing composite coating with a transition layer structure, a preparation method thereof and an application thereof, and belongs to the technical field of wind power generation protective coatings. Background Art

[0002] Icing and icing can pose a serious threat to transportation systems, infrastructure, wind turbines, and many other sectors, potentially leading to severe socioeconomic losses and catastrophic consequences. For example, in the wind energy sector, ice formation on wind turbine blades can cause wind speed measurement errors, power loss, and severely impact the safe and efficient operation of wind farms. Therefore, developing surface engineering technologies that can effectively address icing and icing in extreme environments is of great significance.

[0003] However, some existing coating technologies suffer from poor physical properties, high residual stress between the coating and the substrate, and defects such as bubbles and pores. These problems make the coatings susceptible to erosion and peeling due to rainwater, resulting in insufficient erosion resistance, which limits their widespread adoption in practical applications. To achieve efficient and rapid deicing and improve the anti-icing performance and service life of surfaces such as wind turbine blades, the development of coating materials and preparation processes that combine low ice adhesion strength with high corrosion resistance and durability has become a research priority.

[0004] The present invention aims to provide a composite coating based on the mechanism of introducing a transition layer. By constructing a layered structure and introducing a transition layer, the differences in thermal expansion coefficients and contraction coefficients between different coatings are reduced, and pores or hole defects in the coating preparation process are effectively suppressed, thereby significantly improving the coating's durability and resistance to high-speed rainwater erosion without affecting its hydrophobic / anti-icing properties. The coating design can be used on surfaces such as wind blades to achieve super-hydrophobic and anti-icing functions. In addition, the present invention also provides a method for preparing an anti-icing coating with a simple preparation process, a designable structure, and easy industrial application. The coating prepared by this method has excellent characteristics such as inhibiting ice formation, promoting ice shedding, high mechanical durability, and abrasion resistance, providing an effective solution for anti-icing protection of surfaces such as wind turbine blades. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention provides an anti-icing composite coating with a transition layer structure. A transition layer consisting of an epoxy metal primer coating and a top layer consisting of an epoxy-silicone hybrid resin coating is applied to a blade-shaped substrate. The epoxy-metal primer transition layer enhances interfacial bonding strength, achieves a gradient transition in elastic modulus and thermal expansion coefficient, and significantly improves the adhesion of the top layer, ensuring both good adhesion to the substrate and a compatible fit with the top layer, preventing coating shedding. It also absorbs impact energy, enhancing the composite coating's impact resistance. It also reduces stress concentration, improving the coating's durability and extending its service life. Furthermore, the top layer provides excellent hydrophobicity and anti-icing properties, combining the excellent adhesion of epoxy resin with the low surface energy of silicone resin. Water droplets are less likely to spread on its surface, reducing the contact area and duration between water droplets and the surface, thereby slowing the freezing process and reducing the adhesion between ice and the epoxy-silicone hybrid resin layer. The flexibility provided by the epoxy-silicone hybrid resin allows it to withstand certain deformation and impact. The organic Si component in epoxy resin can reduce the friction coefficient of the coating, reduce the wear caused by friction, and improve the abrasion resistance of the composite coating.

[0006] At the same time, the present invention provides a method for preparing an anti-icing composite coating with a transition layer structure.

[0007] The present invention also provides an anti-icing composite coating with a transition layer structure for use in superhydrophobic / anti-icing applications on engineering components. Once prepared, the anti-icing structure can be applied directly to the surface of certain engineering components to serve as an anti-icing protective layer. It effectively reduces ice adhesion during ice formation, improves deicing efficiency, and reduces energy consumption. The anti-icing coating comprises a multi-gradient system: an epoxy-metal primer coating is sprayed onto the substrate to form a "hard interface," while a top epoxy-silicone hybrid resin coating is cured to form a single layer. This achieves continuous physical property progression from the substrate to the epoxy-metal primer coating and then to the epoxy-silicone hybrid resin coating. The transition layer matches the substrate and exhibits a good elastic modulus transition, preventing sudden interfacial stress and effectively mitigating the negative effects of thermal expansion coefficient mismatches between the different coatings. Simultaneously, the epoxy-metal primer and epoxy-silicone hybrid resin coatings react with epoxy groups to form an interpenetrating network structure. This transition layer resembles a "bionic interface transition zone," mimicking the alternating hard / soft structure of shell nacre. This increases the energy required for crack propagation in the coating and improves the overall performance of the coating system. It is expected to serve fields such as wind energy, aerospace, shipping, and automobiles that need to withstand complex stress and environmental conditions.

[0008] In order to solve the above technical problems, the technical solution adopted by the present invention is: An anti-icing composite coating with a transition layer structure is formed by introducing a premium layer and a top layer, resulting in an anti-icing coating with high strength and resistance to rain erosion. The top layer is made of an epoxy-organic silicone hybrid resin coating, and the substrate is a blade-shaped metal or alloy material.

[0009] The composite coating includes an epoxy-silicone hybrid resin coating, which is modified by introducing glycidoxypropyltrimethoxysilane. The final coating thickness is 150~300μm. The epoxy metal primer coating serving as a transition layer is located between the substrate and the epoxy-silicone hybrid resin coating. The transition layer thickness is 100-200μm. The prepared coating and transition layer must meet the requirements that the end area and the top arc area of the sample are smooth and flat and the thickness distribution is uniform.

[0010] The coating itself is primarily composed of an epoxy-organic silicone hybrid resin, and an epoxy metal primer layer is introduced between the coating and the substrate to improve the coating's adhesion and resistance to high-velocity rainwater erosion. This also reduces the mismatch in elastic modulus and thermal expansion coefficient between the coating and the substrate, reducing pores or holes in the coating preparation process and improving the stability of the coating system. The sample substrate is a leaf-shaped metal or alloy material.

[0011] Glycidoxypropyltrimethoxysilane needs to be added to the epoxy silicone resin coating for modification, and a solvent is added to change the viscosity of the precursor solution so that the thickness distribution of the prepared coating meets the requirements after the brushing process.

[0012] A method for preparing an anti-icing composite coating having a transition layer structure comprises the following steps: Step 1: Prepare the substrate sample and manually polish the sample surface using sandpaper (120-480 grit silicon carbide abrasive sandpaper, Shanghai Chiyong, from low grit to high grit) to maintain a surface roughness of 3.0-3.5 μm. Then, wipe the sample surface with anhydrous ethanol, dry it with a hair dryer, weigh it using an electronic balance, and set aside.

[0013] In step 2, to ensure a smooth, even coating and uniform thickness on the sample surface, and taking into account the viscosity of the precursor solution used, a coating brushing device (consisting of a Newport ESP302 three-axis motion controller with cyclic rotation and a control computer) is used. The sample is mounted on the brushing device, allowing it to maintain continuous, uniform rotation. Taking into account the viscosity of the precursor solution, the precursor solution is prevented from sliding down due to gravity and accumulating at the end of the sample, and the coating brushing device maintains a constant rotation speed throughout the coating process.

[0014] Step 3: Prepare epoxy-organic silicon hybrid resin precursor solution and add it to a plastic container (PP container, for speed mixer) using a rubber-tipped dropper. The epoxy-organic silicon hybrid resin (manufacturer is Dow Inc., specific model is DOWSIL™ 3092 Silicone The two chemicals, epoxy-silicone hybrid resin (Epoxy Silicone Resin) and glycidoxypropyltrimethoxysilane (manufacturer: Shuguang Chemical, specific product model: SG-Si187), are added in a mass ratio of 2 (can fluctuate between 1.9-2.2):0.45 (can fluctuate between 0.42-0.5). After the addition of the two chemicals, a magnetic rotor is added for stirring. The stirring time should start at 12 hours, preferably 16 hours to 24 hours, but not exceed 48 hours. The stirring speed is controlled at 150-250 rpm, and the current viscosity of the mixed solution is evaluated by the movement state of the magnetic rotor. Considering that the epoxy-silicone hybrid resin precursor solution will slowly solidify naturally at room temperature, its solution viscosity will continue to slowly increase. Therefore, if a significant decrease in the magnetic stirring speed is observed, the magnetic stirring speed should be promptly increased. The reference speed after the increase is 250-300 rpm.

[0015] Adding glycidoxypropyltrimethoxysilane to epoxy-organic silicone hybrid resin can increase the hardness of the epoxy-organic silicone hybrid resin and enhance its wear resistance.

[0016] Step 4: About 1 hour before the completion of the precursor solution stirring operation in step 3, start preparing the precursor solution required for the transition layer. The main components are A and B of the epoxy metal primer solution (PPG Amercoat 385 epoxy metal primer from PPG is selected. Component A is mainly a resin base material, including epoxy resin, xylene solvent, and anti-rust pigment, etc. Component B is a curing agent, mainly composed of polyamide and xylene) in a mass ratio of 2.68 (can fluctuate between 2.5-3.0):0.46 (can fluctuate between 0.45-0.6) and placed in a plastic centrifuge tube. Then, use a high-speed mixer to quickly stir and achieve uniformity. During the stirring process, the speed is maintained at 1500-2000 rpm, and multi-stage stirring is performed. Each stirring time is 3-4 minutes, and the number of times is 2-3 times to obtain a uniformly mixed epoxy metal primer solution for standby use.

[0017] Step 5: Secure the blade sample to the horizontal bar of the coating apparatus. The rotation boundary conditions, namely the maximum rotation angle, angular velocity, and number of cycles, are set. Considering the high viscosity of the epoxy metal primer solution required for the transition layer, the rotation angle is set between -100 and +100 degrees, with the sample in an upright position as the origin. The angular velocity is maintained at a constant 10 degrees per second. The dwell time after completing a cycle (returning to the upright position as the origin) is 3 seconds, and the number of cycles is set to 30. The epoxy metal primer is then evenly applied to the sample surface using a flat brush. The brush is then used to smooth the surface, maintaining a relatively smooth and even morphology. The coating thickness is initially monitored by observing the change in mass during the coating process. Once the coating reaches the required thickness (100-200μm), the sample is placed in a forced air drying oven for curing. The curing temperature is set at 48-52°C for 28-32 minutes. After the heat treatment, the sample is removed and weighed. The transition layer structure is prepared and cured.

[0018] Step six, fix the sample obtained in step five on the crossbar of the brushing equipment again. At this time, the epoxy silicone hybrid resin coating precursor solution prepared in step three has been stirred, and its solution viscosity is maintained in a reasonable range (if the precursor solution is brushed on the sample obtained in step 5, the sample is kept in an upright state, and the solution flow rate is about 0.1mm / s at this time). Taking into account the high fluidity of the epoxy silicone hybrid resin coating precursor solution, its rotation angle is adjusted to -120 degrees to +120 degrees, and the rotation angular velocity remains the same as before, maintaining a uniform 10 degrees per second. The residence time after completing one cycle is 8s, and the number of cycles is set to 400-500 times. Use a flat brush head for brushing during the brushing process, and use the brush to re-brush the flowing solution at any time, apply it evenly, and adjust it continuously with the brush. Pay attention to the solution accumulated at the tip of the sample, and clean the pores inside the solution in time to avoid its retention. Keep the thickness distribution from the top to the end of the sample as smooth and uniform as possible, and avoid excessive accumulation in the arc area to cause uneven coating. The quality changes of the brush-applied coating are monitored in real time using an electronic balance. Due to the required thickness, multiple repetitions are required to achieve the desired thickness (150-300μm). The sample is then removed and transferred to a forced air drying oven for curing. The heating method uses a combination of furnace-based heating and gradient heating: first, the coating is treated at 33-37°C for 3.5-4.5 hours, then raised to 53-57°C for another 3.5-4.5 hours, then to 73-77°C for 3.5-4.5 hours, and finally to 108-112°C for 15-17 hours. Throughout this process, the heating rate is maintained at 1°C / min to prevent cracks on the sample surface due to rapid heating. After the heating cycle is completed, the forced air drying oven is closed and the sample is allowed to cool with the furnace. Once cooled to room temperature, the sample is removed and weighed.

[0019] The gradient heating process can effectively eliminate thermal stress concentration, reduce possible defects inside the coating, and avoid large internal temperature differences caused by rapid heating and deformation, cracks or coating cracking caused by thermal stress. In addition, the gradient heating process can optimize the curing process of epoxy-silicone hybrid resins, control their cross-linking reaction rate, and avoid increased brittleness caused by local over-curing. Thirdly, the gradient heating process can improve the adhesion and density of the coating / plating, making the curing more thorough, reducing the porosity of the coating, and improving the bonding strength with the substrate. Finally, the gradient heating process can ensure the consistency of the overall performance of the coating, prevent the coating surface from curing prematurely while the interior has not yet fully reacted, affecting the volatilization of the internal solvent. Moreover, the gradient heating process can effectively widen the process window and is suitable for some complex workpieces or sensitive materials.

[0020] In step 3, the epoxy-silicone hybrid resin for the top coating was prepared using DOWSIL™ 3092 Silicone Resin and the corresponding hardener 3-aminopropyltrimethoxysilane (APTMS). The ratio of DOWSIL™ 3092 Silicone Resin to APTMS is 2:0.45. Add both to the container sequentially using a rubber-tipped dropper and stir thoroughly for 16-24 hours. Continue stirring until the solution reaches a high viscosity before proceeding to the next step.

[0021] In step six, brushing the top coat is more challenging due to its high viscosity, so a flat brush head is recommended, not a rounded one. The sample weight should be recorded before and after brushing. For the second curing step, gradient heating is required to prevent uneven heating of the coating and cracking.

[0022] In step six, the epoxy-silicone hybrid resin precursor solution cannot be applied immediately after stirring. It must first be transferred to a vacuum box for vacuum degassing at a vacuum degree of 0.05-0.08 atmospheres for 10-20 minutes to remove bubbles in the solution.

[0023] In step 6, the determined number of cycles of 400-500 times is not a limit value and can be adjusted according to the required coating thickness requirements.

[0024] The preparation method of the present invention can be used for samples of various regular or irregular shapes.

[0025] Compared with the prior art, the present invention has the following beneficial effects: This invention utilizes a composite anti-icing coating with a transition layer structure and its preparation method to enhance its anti-icing performance and durability. By introducing an epoxy metal primer as a transition layer, connecting the substrate with the epoxy-organic silicone hybrid resin top layer, a composite coating system with a gradient modulus and excellent interfacial bonding is formed. This improves coating adhesion and enhances its anti-icing performance.

[0026] The present invention addresses the problem that some anti-icing coatings in the prior art are difficult to achieve both durability and efficient de-icing capabilities, and proposes a composite coating design strategy based on a transition layer structure. By introducing an epoxy metal primer transition layer, the interfacial bonding strength between the coating and the substrate is enhanced, and a gradient transition of the elastic modulus and thermal expansion coefficient is achieved. The rough structure of the epoxy metal primer transition layer can provide a mechanical anchor point for the top coating, thereby effectively improving the adhesion of the top coating, allowing it to remain stable for a long time under the impact of high-speed water flow. At the same time, its hydrophobicity can be sustained and stable, and the static water contact angle can always be maintained above 110 degrees. At the same time, the contact angle hysteresis is less than 5 degrees, and the rolling angle is less than 10 degrees, so that it can not only be well bonded to the substrate, but also match the top coating, preventing and delaying the shedding of the coating during service. The epoxy-silicone hybrid resin in the top coating combines the high adhesion of epoxy with the low surface energy of silicone. This ensures chemical covalent bonding with the intermediate layer, slowing the freezing process. It also allows the siloxane chains in the coating to rotate and strengthen at low temperatures, reducing the adhesion between ice and the coating surface, lowering the ice adhesion strength to below 20 kPa. This in turn improves the anti-icing and abrasion resistance of the composite coating. The anti-icing coating prepared using this method exhibits efficient deicing capabilities and excellent mechanical durability.

[0027] The present invention adopts a brush coating method, which has simple process, is easy to operate, has the feasibility of large-scale production, and can relatively easily realize the preparation of an anti-icing structure with anti-icing capability and durability.

[0028] The present invention discloses a composite anti-icing coating with a transition layer structure, which offers both high abrasion resistance and anti-icing performance. The coating comprises a blade-shaped sample substrate with a two-layer composite structure formed on its surface: a first transition layer, an epoxy metal primer coating, and a second, top layer, an epoxy-organic silicone hybrid resin coating. The present invention also discloses a preparation method and application of the composite anti-icing coating with a transition layer structure, which effectively inhibits ice formation and promotes ice shedding. The coating obtained by the present invention incorporates a transition layer mechanism to reduce mismatches in elastic modulus and thermal expansion coefficient between different coatings without affecting the coating's hydrophobicity / anti-icing capabilities. It also reduces pores or holes that may occur during the coating preparation process, resulting in high mechanical durability and abrasion resistance, significantly improving its resistance to high-speed water erosion. The method provided by the present invention utilizes readily available and inexpensive raw materials for the coating preparation, and the preparation process is simple and straightforward. Furthermore, the coating exhibits excellent hydrophobicity, deicing properties, and high mechanical durability, showing promising application prospects in anti-icing applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The substrate sample used in Example 1 of the present invention is a sample having a leaf shape; Figure 2 The coating brushing device used in Example 1 of the present invention; Figure 3 This is a normal photo of Example 1 of the present invention; Figure 4 3D contour image of the sample substrate after sandpaper polishing used in Example 1 of the present invention; Figure 5 These are SEM images of Example 1 of the present invention, where (a) shows the surface of the sample after the transition layer of epoxy metal primer is applied; (b) shows the surface after the top layer of epoxy silicone hybrid resin coating is applied; Figure 6 This is a static water contact angle diagram measured for the composite anti-icing coating of Example 1 of the present invention; Figure 7 The ice bonding strength results of Example 1 of the present invention and the sample substrate after sandpaper polishing; Figure 8 The time taken for Example 1 of the present invention and Comparative Example 1 to finally rupture after the high-speed water impact test; Figure 9 This is a common photo of Comparative Example 2 of the present invention. DETAILED DESCRIPTION

[0030] The present invention will be further described in detail below with reference to the accompanying drawings and specific examples. The following examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. Example 1

[0031] This embodiment provides a method for preparing a super-hydrophobic / anti-icing composite coating with a transition layer structure and good durability, comprising the following steps: Step 1: Prepare leaf samples (e.g. Figure 1 The blade sample surface was manually polished using 120-grit, 240-grit, and 360-grit sandpaper (silicon carbide abrasive sandpaper, Shanghai Chiyong) to make the sample surface roughness 3.1 ± 0.2 μm (as shown). Figure 4 As shown), the polished sample surface was then wiped with anhydrous ethanol, dried with a hair dryer, weighed with an electronic balance, and set aside.

[0032] Step 2: To ensure that the sample surface coating is smooth and uniform in thickness, and taking into account the viscosity of the precursor used, use Figure 2The coating brush coating device shown (composed of a periodically rotatable motion controller and a control computer) mounts the sample on the brush coating device so that the sample can maintain continuous uniform rotation. Taking into account the viscosity of the precursor solution, the precursor solution will not slide down due to gravity and accumulate in the end area of the sample, and the sample will always maintain a uniform rotation during the coating brush coating process.

[0033] Step 3: Prepare an epoxy-silicone hybrid resin precursor solution and add it to a plastic container (PP container, for speed mixer) using a rubber-tipped dropper. The epoxy-silicone hybrid resin and glycidoxypropyltrimethoxysilane are added in a mass ratio of 2:0.45. After the addition of the two chemicals, add a magnetic rotor for stirring. The stirring time is 24 hours, and the stirring speed is controlled at 200 rpm. The movement state of the magnetic rotor is observed every 4 hours to evaluate the current viscosity of the mixed solution. When the magnetic speed is observed to decrease, the magnetic stirring speed is promptly increased to 300 rpm.

[0034] Step 4. About 1 hour before the completion of the precursor solution stirring operation in step 3, start preparing the precursor solution required for the transition layer. Its main components are the two parts A and B of the epoxy metal primer solution placed in a plastic centrifuge tube in a mass ratio of 2.68:0.46, and then use a high-speed mixer to quickly stir and achieve uniformity. The stirring process speed is 2000 rpm, the stirring time is 3 minutes, and the number of times is 3 times to obtain a uniformly mixed epoxy metal primer solution, which is set aside.

[0035] Step 5: Secure the blade sample to the horizontal bar of the coating equipment. The rotation boundary conditions, namely the maximum rotation angle, angular velocity, and number of cycles, are set. Considering the high viscosity of the epoxy metal primer solution required for the transition layer, the rotation angle is set between -100 and +100 degrees, the angular velocity is maintained at a uniform 10 degrees per second, the cooling time after each cycle is 3 seconds, and the number of cycles is set to 30. The epoxy metal primer is then evenly applied to the sample surface using a flat brush. The brush is then used to smooth the surface, maintaining a relatively smooth and even morphology. The coating thickness is initially measured by the mass change during the coating process. After coating, the sample is placed in a forced air drying oven for curing. The curing temperature is set at 50°C and the holding time is 30 minutes. After the heat treatment, the sample is removed and weighed. Based on the mass change and the coating's density, the thickness of the epoxy metal primer layer, serving as the transition layer, is calculated to be approximately 200 μm.

[0036] Step six, fix the sample obtained in step five on the crossbar of the brushing equipment again. At this time, the epoxy silicone hybrid resin coating precursor solution prepared in step three has been stirred, and its solution viscosity is maintained in a reasonable range (at this time, the solution is brushed on the sample obtained in step five, the sample is in an upright state, and the solution flow rate is 0.1mm / s). Taking into account the high fluidity of the epoxy silicone hybrid resin coating precursor solution, the sample rotation angle is -120 degrees to +120 degrees, the rotation angular velocity is kept uniform, which is 10 degrees per second, the residence time after completing one cycle is 8s, and the number of cycles is set to 500 times. Use a flat brush head for brushing during the brushing process, and use the brush to re-brush the flowing solution at any time, apply it evenly, and adjust it continuously with the brush. Pay attention to the solution accumulated at the tip of the sample, and clean the pores inside the solution in time to avoid its retention. Keep the thickness distribution from the top to the end of the sample as smooth and uniform as possible, and avoid excessive accumulation in the arc area to cause uneven coating. The mass change of the brush-applied coating was monitored in real time using an electronic balance. Due to the required thickness, the process required repeated multiple times to achieve the desired thickness. The sample was then removed and placed in a blast drying oven for curing. A gradient heating method was used: first, the coating was treated at 35°C for 4 hours, then raised to 55°C for another 4 hours, then to 75°C for 4 hours, and finally to 110°C for 16 hours. The heating rate was maintained at 1°C / min throughout the entire process to prevent cracks on the sample surface due to excessively rapid heating. After the heating cycle was completed, the blast drying oven was closed and the sample was allowed to cool in the furnace. When it cooled to room temperature, the sample was removed and weighed. Based on the mass change and the coating's density, the thickness of the epoxy-silicone hybrid resin coating, which serves as the top layer, was calculated to be approximately 250 μm.

[0037] A multi-layer composite anti-icing structure with good deicing performance and durability based on the introduction of a transition layer is used on the surface of engineering components. The engineering components include those with irregular surfaces that require anti-icing operations, including wind turbine blades. After the composite anti-icing coating structure is prepared, its main purpose is to directly act as an anti-icing protective layer on the surface of the engineering component and to improve its anti-abrasion ability. At the same time, it optimizes the deicing efficiency of the deicing process dominated by external forces. The prepared anti-icing structure can first effectively drive away supercooled droplets on the surface and delay the freezing of supercooled droplets.

[0038] An anti-icing composite coating with a transition layer structure comprises a base, a transition layer, and a top layer. The base is a blade-shaped metal or alloy material; the transition layer is an epoxy metal primer coating; and the top layer is an epoxy-organosilicon hybrid resin coating. The transition layer is 200 μm thick; the top layer is 250 μm thick; and the base surface roughness is maintained at 3.1 ± 0.2 μm.

[0039] Comparative Example 1

[0040] The difference between this comparative example and Example 1 is that the thickness of the epoxy metal primer layer prepared as the transition layer in step 5 is about 80 μm, the number of cycles in step 6 is set to 400 times, and the thickness of the epoxy silicone hybrid resin coating prepared as the top layer is about 200 μm. The rest is the same as the specific embodiment 1.

[0041] Comparative Example 2

[0042] The difference between this comparative example and Example 1 is that in step 6, the blast drying oven can be replaced with a vacuum oven, and a vacuum method (0.5 atmospheres) is used during the heating and curing process. The rest is the same as the specific embodiment 1. Since a vacuum heating method is used during the curing process, many bubbles appear on the surface of the sample, which seriously affects the quality of the sample. The top coating will be cured first under the action of high temperature, and a dense structure will be formed on the surface, which will limit the release of gas during the curing process of the internal coating. However, the vacuum degree in the vacuum oven chamber is relatively low, resulting in a pressure difference between the inside and the outside, which will cause the coating to rupture, forming the following Figure 9 The blistering is shown. The outer coating cures first, preventing gas release from the inner coating during curing. This restricts gas release from the inner coating during curing. These pores in the coating become defects, easily rupturing when subjected to high-velocity water impact, leading to coating failure.

[0043] Comparative Example 3

[0044] The difference between this comparative example and Example 1 is that the gradient heating method in the curing process in step six is: first, treat at 30°C for 4 hours, then heat to 60°C, continue to treat for 4 hours, then heat to 80°C for 4 hours, and finally heat to 100°C for 16 hours. The heating rate during the whole process is maintained at 1°C / min. The rest is the same as Example 1.

[0045] Relevant characterization and testing methods of the coating of the present invention: (1) Photography with a regular camera and surface 3D topography analysis: The macroscopic morphology of the prepared anti-icing coating was photographed using an ordinary camera, and its surface roughness and 3D morphological characteristics were measured using a 3D profilometer (UP-3000) non-contact optical profilometer.

[0046] (2) Scanning electron microscopy analysis: The surface microstructure of the prepared anti-icing coating was characterized using a JSM-6360LV SEM, scanning at a voltage of 20 kV and a working distance of 10 mm. Because the epoxy metal primer and epoxy-silicone hybrid resin coatings are not electrically conductive, they were treated with a platinum spray prior to imaging. This added a thin layer of platinum (Pt) to make the coating conductive and facilitate imaging. Given the large sample size, a small sample was cut for subsequent SEM observation when performing various surface characterization techniques.

[0047] (3) Static water contact angle test: The surface wettability of the coating material was tested using an optical contact angle meter (JY-82C). The test solvent was deionized water, the test droplet volume was 5µL, the release rate was 1µL / s, and 5 locations were selected for testing on each sample, and the average value was calculated.

[0048] (4) Ice bonding strength test: Measurements are performed using the centrifugation method in a -10°C environmental chamber. A prepared sample / ice cube and a counterweight of equal mass are placed at either end of a rod and subjected to rotational acceleration. As the rod accelerates, the sample also maintains centripetal acceleration. When the centrifugal force exceeds the ice bond strength between the sample and the ice cube, the sample separates from the ice cube, and the ice cube is ejected. The ice bond strength of the sample can then be calculated based on the ice mass, rod length, and test duration.

[0049] (5) High-speed water flow impact test: The prepared sample was secured to a fixture and placed parallel to and 80 cm horizontally from a nozzle (nozzle diameter 2.5 mm). Under the influence of compressed air at 2.1 atmospheres, water was ejected from the nozzle at a velocity of 67 m / s, directly impacting the sample surface (the liquid flow rate upon exiting the nozzle was calculated to be 2.5 mL / s). The entire scouring test was a staged process, with each scouring lasting 10 seconds. The experiment was then stopped, the sample surface observed, and then restarted, repeating this cycle until the sample surface was damaged. After the experiment, the effects of high-speed water scouring on the coating surface morphology were investigated.

[0050] (6) Energy consumed by coating crack propagation: The energy consumed by crack propagation is mainly affected by the intrinsic fracture energy of epoxy resin and the toughening mechanism of interpenetrating network structure.

[0051] The fracture energy of the epoxy-silicone interpenetrating network structure of the present invention is about 1500 J / m 2 (Better than pure epoxy, but lower than pure elastomer).

[0052] When the fracture energy of different components of the interpenetrating network structure is known, the energy consumed by the coating crack propagation is approximated, and the specific formula is G C,IPN ≈ φ 环氧 G C,环氧 + φ 有机硅 G C,有机硅 +ΔG 界面 , where φ is the volume fraction; ΔG 界面 Add energy to the interfacial interactions.

[0053]

[0054] Here, γ is the surface energy. The surface energy of both epoxy (i.e., epoxy resin in epoxy metal primer) and silicone (i.e., epoxy-silicone hybrid resin) can be measured using the Owens-Wendt method.

[0055] The test method or test standard for the energy consumed by crack propagation: Using the fracture toughness test (ASTM D5045), using a single-edge notched beam specimen, measure the critical stress intensity factor K IC , and then converted to Gc, ,in, E’ is the effective modulus, , E’ Mainly used to correct the elastic modulus under plane strain conditions E , E is the elastic modulus of the material itself, v is the Poisson's ratio of the material.

[0056] That is G C,环氧 , G C,有机硅 All are calculated using the above formula.

[0057] (7) Coating porosity: Scanning electron microscopy image analysis was performed using the ASTM E2809 standard. The coating cross section was treated with Pt spraying and observed using a scanning electron microscope. Photos were obtained and the percentage of pore area was calculated using ImageJ software. Multiple images were averaged.

[0058] Figure 1 The substrate sample used in Example 1 is shown. It can be seen that the substrate is semi-elliptical in shape, with an overall width of 28.0 mm, a sample height of 40.0 mm, and a sample length of 450.0 mm. The sample has a smooth transition from the top to the lower end area.

[0059] Figure 2The coating brush application apparatus used in Example 1 of the present invention is provided. It primarily comprises a control computer, a cyclically rotatable motion controller, a rotating rod, and a sample. With the sample in an upright position as the origin, the rotation angle can range from -180 degrees to +180 degrees, maintaining a uniform angular velocity.

[0060] Figure 3 A general photo of Example 1 of the present invention is given, wherein the gray coating is an epoxy metal primer and the top coating is a transparent epoxy silicone hybrid resin, but Figure 3 It is not obvious from the observation in the middle, and it can be seen that the bottom coating and the top coating are evenly distributed on the sample surface and adhere well and tightly.

[0061] Figure 4 A 3D profile photograph of the surface of the substrate used in Example 1 of the present invention obtained by a 3D profilometer after sandpaper polishing is shown, and the surface roughness is 3.1±0.2 μm.

[0062] Figure 5 SEM images of Example 1 of the present invention are provided. (a) shows the surface of the sample after applying a transition layer of epoxy metal primer. The surface is very smooth and flat, with almost no defects or holes. (b) shows the surface after applying a top layer of epoxy-organic silicone hybrid resin coating. Although the surface has some wrinkles, it still appears flat overall.

[0063] Figure 6 The static water contact angle of the composite anti-icing coating obtained in Example 1 is measured and is 124.4±2.3°, indicating a surface hydrophobic characteristic.

[0064] Figure 7 The ice adhesion strength of Example 1 and a sandpaper-polished sample substrate is shown. The ice adhesion strength of Example 1 is a relatively low 15.6 ± 2.1 kPa, reflecting the composite coating's excellent deicing capabilities. For comparison, the ice adhesion strength of the polished substrate is 112.7 ± 4.5 kPa. This demonstrates that the introduction of the coating effectively reduces ice adhesion strength. While Example 1 effectively improves the durability of the anti-icing structure through the introduction of the composite coating structure, it also achieves lower ice adhesion strength, ensuring excellent deicing capabilities.

[0065] Figure 8The following table compares the duration of surface integrity maintenance of the coating samples of Example 1 and Comparative Example 1 under conditions of sustained high-speed water flow. It can be seen that Example 1 maintained surface integrity for 680 seconds under high-speed water flow, demonstrating the excellent durability of the coating. Comparative Example 1, used as a reference, maintained surface integrity for 490 seconds. This demonstrates that the introduction of a transition layer effectively improves the stability of the composite coating structure. In particular, increasing the thickness of the transition layer significantly enhances the coating's durability and abrasion resistance.

[0066] In Comparative Example 3, the energy required for crack propagation was approximately 1000 J / m². The echelon heating process facilitated uniform crosslinking of the epoxy and silicone networks, forming a denser interpenetrating network. The energy required for crack propagation in Comparative Example 1 was 750 J / m². In contrast, the energy required for crack propagation in Example 1 was approximately 1500 J / m². Therefore, the present invention increases the energy required for crack propagation in the coating, improving the overall performance of the coating system. This technology is expected to serve applications in wind energy, aerospace, shipbuilding, automotive, and other fields that must withstand complex stresses and environmental conditions.

[0067] Coating porosity: The coating porosity of Comparative Example 1 is about 1.2%, with pore size less than 50 nm. The coating porosity of Comparative Example 3 is about 3.3%, and the coating porosity of Example 1 is about 0.8%.

[0068] The gradient heating process of this invention is suitable for workpieces with complex geometries, preventing thermal stress cracking that can be caused by rapid, uniform heating. Alternatively, for workpieces with significantly different expansion coefficients, gradient heating can prevent interfacial debonding caused by sudden heating. Furthermore, for applications sensitive to residual stress, gradient heating can eliminate processing stresses and prevent deformation.

[0069] In particular, the gradient temperature ramp process in this invention prevents premature gelation of the epoxy system and ensures uniform formation of the siloxane network. This gradient temperature ramp activates different reactions in stages. The low-temperature stage prioritizes the reaction between epoxy groups and the curing agent, forming preliminary crosslinks. The intermediate-temperature stage accelerates the hydrolysis and condensation of the siloxane, allowing interpenetration with the epoxy network. The higher-temperature stage allows for the completion of the reaction of residual groups, enhancing the density of the interpenetrating network structure. Example 2

[0070] A method for preparing an anti-icing composite coating having a transition layer structure comprises the following steps: Step 1: Prepare the blade sample and manually polish the surface of the blade sample using 120-mesh, 240-mesh, 360-mesh, and 480-mesh sandpaper (silicon carbide abrasive sandpaper, Shanghai Chiyong) to make the surface roughness of the sample 3.5 μm. Then, wipe the polished sample surface with anhydrous ethanol and blow dry it with a hair dryer. Weigh it using an electronic balance and set it aside.

[0071] Step 2: To ensure that the coating on the sample surface is smooth and even with uniform thickness, and taking into account the viscosity of the precursor used, a coating brushing device (consisting of a motion controller and a control computer that can rotate periodically) is used to install the sample on the brushing device so that the sample can maintain continuous uniform rotation. Taking into account the viscosity of the precursor solution, the precursor solution will not slide due to gravity and accumulate in the end area of the sample, and will always maintain a uniform rotation during the coating brushing process.

[0072] Step 3: Prepare the epoxy-silicone hybrid resin precursor solution and add it to a plastic container (PP container, for speed mixer) using a rubber-tipped dropper. The epoxy-silicone hybrid resin and glycidoxypropyltrimethoxysilane are added in a mass ratio of 1.9:0.42. After the addition of the two chemicals, add a magnetic rotor for stirring. The stirring time is 16 hours, and the stirring speed is controlled at 150 rpm. The movement state of the magnetic rotor is observed every 4 hours to evaluate the current viscosity of the mixed solution. When the magnetic speed is observed to decrease, the magnetic stirring speed is promptly increased to 250 rpm.

[0073] Step 4. About 1 hour before the completion of the precursor solution stirring operation in step 3, start preparing the precursor solution required for the transition layer. Its main components are the two parts A and B of the epoxy metal primer solution placed in a plastic centrifuge tube in a mass ratio of 2.5:0.45, and then use a high-speed mixer to quickly stir and achieve uniformity. The stirring process speed is 1500 rpm, the stirring time is 4 minutes, and the number of times is 2 times to obtain a uniformly mixed epoxy metal primer solution, which is set aside.

[0074] In step five, the blade sample is secured to the horizontal bar of the coating apparatus. The rotation boundary conditions, namely the maximum rotation angle, angular velocity, and number of cycles, are set. Considering the high viscosity of the epoxy metal primer solution required for the transition layer, the rotation angle is set between -100 and +100 degrees, the angular velocity is maintained at a uniform 10 degrees per second, the cooling time after each cycle is 3 seconds, and the number of cycles is set to 30. The epoxy metal primer is then evenly applied to the sample surface using a flat brush. The brush is then used to smooth the surface, maintaining a relatively smooth and even morphology. The coating thickness is initially measured by the mass change during the coating process. After coating, the sample is placed in a forced air drying oven for curing. The curing temperature is set at 48°C and the holding time is 28 minutes. After the heat treatment, the sample is removed and weighed. Based on the mass change and the coating's density, the thickness of the epoxy metal primer layer, serving as the transition layer, is calculated to be approximately 100 μm.

[0075] Step six, fix the sample obtained in step five on the crossbar of the brushing equipment again. At this time, the epoxy silicone hybrid resin coating precursor solution prepared in step three has been stirred, and its solution viscosity is maintained in a reasonable range (at this time, the solution is brushed on the sample obtained in step five, the sample is in an upright state, and the solution flow rate is 0.1mm / s). Taking into account the high fluidity of the epoxy silicone hybrid resin coating precursor solution, the sample rotation angle is -120 degrees to +120 degrees, the rotation angular velocity is kept uniform, which is 10 degrees per second, the residence time after completing one cycle is 8s, and the number of cycles is set to 400 times. Use a flat brush head for brushing during the brushing process, and use the brush to re-brush the flowing solution at any time, apply it evenly, and adjust it with the brush continuously, pay attention to the solution accumulated at the tip of the sample, and clean the pores inside the solution in time to avoid its retention. Keep the thickness distribution from the top to the end of the sample as smooth and uniform as possible, and avoid excessive siltation in the arc area to cause uneven coating. The mass change of the brush-applied coating was monitored in real time using an electronic balance. Due to the required thickness, the process required multiple repetitions to achieve the desired thickness. The sample was then removed and placed in a convection drying oven for curing. A gradient heating method was used: curing was first performed at 33°C for 3.5 hours, then ramped up to 53°C for another 3.5 hours, then to 73°C for another 3.5 hours, and finally to 108°C for 15 hours. The heating rate was maintained at 1°C / min throughout the entire process to prevent cracks on the sample surface caused by excessive heating. After the heating cycle, the convection drying oven was closed and the sample was allowed to cool in the furnace. Once cooled to room temperature, the sample was removed and weighed. Based on the mass change and the coating's density, the thickness of the top epoxy-silicone hybrid resin coating was calculated to be approximately 150 μm.

[0076] A multi-layer composite anti-icing structure with good deicing performance and durability based on the introduction of a transition layer is used on the surface of engineering components. The engineering components include those with irregular surfaces that require anti-icing operations, including wind turbine blades. After the composite anti-icing coating structure is prepared, its main purpose is to directly act as an anti-icing protective layer on the surface of the engineering component and to improve its anti-abrasion ability. At the same time, it optimizes the deicing efficiency of the deicing process dominated by external forces. The prepared anti-icing structure can first effectively drive away supercooled droplets on the surface and delay the freezing of supercooled droplets.

[0077] An anti-icing composite coating with a transition layer structure includes a base, a transition layer, and a top layer. The base is a blade-shaped metal or alloy material; the transition layer is an epoxy metal primer coating; and the top layer is an epoxy-organosilicon hybrid resin coating. The transition layer is 100 μm thick; the top layer is 150 μm thick; and the base surface roughness is maintained at 3.5 μm. Example 3

[0078] This embodiment provides a method for preparing a super-hydrophobic / anti-icing composite coating with a transition layer structure and good durability, comprising the following steps: Step 1: Prepare the blade sample and manually polish the surface of the blade sample using 120-mesh, 240-mesh, and 360-mesh sandpaper (silicon carbide abrasive sandpaper, Shanghai Chiyong) to make the surface roughness of the sample 3.0 μm. Then, wipe the polished sample surface with anhydrous ethanol and blow dry it with a hair dryer. Weigh it using an electronic balance and set it aside for later use.

[0079] Step 2: To ensure that the coating on the sample surface is smooth and even with uniform thickness, and taking into account the viscosity of the precursor used, a coating brushing device (consisting of a motion controller and a control computer that can rotate periodically) is used to install the sample on the brushing device so that the sample can maintain continuous uniform rotation. Taking into account the viscosity of the precursor solution, the precursor solution will not slide due to gravity and accumulate in the end area of the sample, and will always maintain a uniform rotation during the coating brushing process.

[0080] Step 3: Prepare an epoxy-silicone hybrid resin precursor solution and add it to a plastic container (PP container, for speed mixer) using a rubber-tipped dropper. The epoxy-silicone hybrid resin and glycidoxypropyltrimethoxysilane are added in a mass ratio of 2.2:0.5. After the addition of the two chemicals, add a magnetic rotor for stirring. The stirring time is 24 hours, and the stirring speed is controlled at 250 rpm. The movement state of the magnetic rotor is observed every 4 hours to evaluate the current viscosity of the mixed solution. When the magnetic speed is observed to decrease, the magnetic stirring speed is promptly increased to 300 rpm.

[0081] Step 4. About 1 hour before the completion of the precursor solution stirring operation in step 3, start preparing the precursor solution required for the transition layer. Its main components are the two parts A and B of the epoxy metal primer solution placed in a plastic centrifuge tube in a mass ratio of 3.0:0.6, and then use a high-speed mixer to quickly stir and achieve uniformity. The stirring process speed is 2000 rpm, the stirring time is 3 minutes, and the number of times is 3 times to obtain a uniformly mixed epoxy metal primer solution, which is set aside.

[0082] In step five, the blade sample is secured to the horizontal bar of the coating apparatus. The rotation boundary conditions, namely the maximum rotation angle, angular velocity, and number of cycles, are set. Considering the high viscosity of the epoxy metal primer solution required for the transition layer, the rotation angle is set between -100 and +100 degrees, the angular velocity is maintained at a uniform 10 degrees per second, the cooling time after each cycle is 3 seconds, and the number of cycles is set to 30. The epoxy metal primer is then evenly applied to the sample surface using a flat brush. The brush is then used to smooth the surface, maintaining a relatively smooth and even morphology. The coating thickness is initially measured by the mass change during the coating process. After coating, the sample is placed in a forced air drying oven for curing. The curing temperature is set at 52°C and the holding time is 32 minutes. After the heat treatment, the sample is removed and weighed. Based on the mass change and the coating's density, the thickness of the epoxy metal primer layer, serving as the transition layer, is calculated to be approximately 200 μm.

[0083] Step six, fix the sample obtained in step five on the crossbar of the brushing equipment again. At this time, the epoxy silicone hybrid resin coating precursor solution prepared in step three has been stirred, and its solution viscosity is maintained in a reasonable range (at this time, the solution is brushed on the sample obtained in step five, the sample is in an upright state, and the solution flow rate is 0.1mm / s). Taking into account the high fluidity of the epoxy silicone hybrid resin coating precursor solution, the sample rotation angle is -120 degrees to +120 degrees, the rotation angular velocity is kept uniform, which is 10 degrees per second, the residence time after completing one cycle is 8s, and the number of cycles is set to 500 times. Use a flat brush head for brushing during the brushing process, and use the brush to re-brush the flowing solution at any time, apply it evenly, and adjust it continuously with the brush. Pay attention to the solution accumulated at the tip of the sample, and clean the pores inside the solution in time to avoid its retention. Keep the thickness distribution from the top to the end of the sample as smooth and uniform as possible, and avoid excessive accumulation in the arc area to cause uneven coating. The mass change of the brush-applied coating is monitored in real time by weighing on an electronic balance. Due to the required thickness, the operation needs to be repeated many times to finally reach the required thickness. The sample is then removed and moved into a blast drying oven for curing. The heating method adopts a gradient heating method. First, it is treated at 37°C for 4.5 hours, then the temperature is raised to 57°C for another 4.5 hours, then the temperature is raised to 77°C for 4.5 hours, and finally the temperature is raised to 112°C for 17 hours. The heating rate is kept at 1°C / min throughout the process to prevent cracks on the sample surface due to excessive heating rate. After the heating step is completed, the blast drying oven is turned off and cooled with the furnace. When it cools to room temperature, the sample is taken out and weighed. According to the mass change and the density of the coating itself, the thickness of the epoxy-silicone hybrid resin coating as the top layer is calculated to be approximately 300μm.

[0084] A multi-layer composite anti-icing structure with good deicing performance and durability based on the introduction of a transition layer is used on the surface of engineering components. The engineering components include those with irregular surfaces that require anti-icing operations, including wind turbine blades. After the composite anti-icing coating structure is prepared, its main purpose is to directly act as an anti-icing protective layer on the surface of the engineering component and to improve its anti-abrasion ability. At the same time, it optimizes the deicing efficiency of the deicing process dominated by external forces. The prepared anti-icing structure can first effectively drive away supercooled droplets on the surface and delay the freezing of supercooled droplets.

[0085] An anti-icing composite coating with a transition layer structure includes a base, a transition layer, and a top layer. The base is a blade-shaped metal or alloy material; the transition layer is an epoxy metal primer coating; and the top layer is an epoxy-organosilicon hybrid resin coating. The transition layer is 200 μm thick; the top layer is 300 μm thick; and the base surface roughness is maintained at 3.0 μm.

[0086] It should be understood that in order to streamline the present disclosure and aid understanding of one or more of the various inventive aspects, in the above description of exemplary embodiments of the invention, various features of the invention are sometimes grouped together into a single embodiment, figure, or description thereof. However, this disclosed method should not be interpreted as reflecting an intention that the claimed invention requires more features than are expressly recited in each claim. Rather, as reflected in the claims, inventive aspects lie in less than all of the features of the previously disclosed embodiments. Accordingly, the claims that follow the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of the invention.

[0087] Although the present invention has been described with respect to a limited number of embodiments, it will be apparent to those skilled in the art, having benefit of the foregoing description, that other embodiments are contemplated within the scope of the invention thus described. Furthermore, it should be noted that the language used in this specification has been selected primarily for readability and didactic purposes, rather than for the purpose of explaining or limiting the subject matter of the present invention. Consequently, many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the appended claims. The disclosure of the present invention is intended to be illustrative rather than restrictive of the scope of the invention, which is defined by the appended claims.

[0088] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. An anti-icing composite coating with a transition layer structure, characterized in that: including a base, a transition layer and a top layer introduced on the base; The base material is metal or alloy material; The transition layer is an epoxy metal primer coating; The top layer is an epoxy-silicone hybrid resin coating.

2. The anti-icing composite coating with a transition layer structure according to claim 1, characterized in that: The thickness of the transition layer is 100-200μm; the thickness of the top layer is 150~300μm.

3. The anti-icing composite coating with a transition layer structure according to claim 1, characterized in that: The substrate surface roughness was maintained at 3.0-3.5 μm.

4. The method for preparing an anti-icing composite coating having a transition layer structure according to any one of claims 1 to 3, characterized in that: The following steps are involved: Step 1, pre-treating the substrate sample; Step 2: Mount the pre-treated substrate sample on a brush coating device that can maintain a constant rotation speed; Step 3: Prepare an epoxy-silicone hybrid resin precursor solution, add epoxy-silicone hybrid resin and glycidoxypropyltrimethoxysilane dropwise into a plastic container in a mass ratio of (1.9-2.2): (0.42-0.5), and stir after the two chemicals are added. The stirring time is 16h-24h, and the stirring speed is controlled at 150-250rpm. When the stirring speed drops to <150rpm due to the increase in viscosity of the epoxy-silicone hybrid resin precursor solution, the stirring speed is increased to 250-300rpm. Step 4: Before the stirring operation of the epoxy-organic silicone hybrid resin precursor solution in step 3 is completed, the precursor solution required for the transition layer is prepared. Parts A and B of the epoxy metal primer solution are placed in a plastic centrifuge tube in a mass ratio of (2.5-3.0): (0.45-0.6), and then stirred at a speed of 1500-2000 rpm. Multi-stage stirring is performed, with each stirring time being 3-4 minutes and repeated 2-3 times to obtain a uniformly mixed epoxy metal primer solution, which is set aside for later use. Step 5: Fix the substrate sample to the crossbar of the brush coating equipment, take the upright state of the substrate sample as the origin, set the rotation angle to -100 degrees to +100 degrees, keep the rotation angular velocity uniform at 10 degrees per second, the dwell time after completing one cycle is 3 seconds, and the number of cycles is set to 30 times; then use a flat brush to evenly brush the epoxy metal primer on the surface of the substrate sample. After the brushing is completed, place the sample in a blast drying oven for curing treatment. The curing temperature is set at 48-52°C and the heat preservation time is 28-32 minutes. After the heat treatment is completed, take it out immediately to obtain the transition layer; Step 6: Fix the sample obtained in step 5 on the crossbar of the brush coating equipment again. At this time, the epoxy silicone hybrid resin precursor solution prepared in step 3 has been stirred, the rotation angle is adjusted to -120 degrees to +120 degrees, the rotation angular velocity is kept uniform at 10 degrees per second, the residence time after completing one cycle is 8 seconds, and the number of cycles is set to 400-500 times; use a flat brush head for brushing during the brushing process. After brushing, remove the sample and move it into a blast drying oven for curing. The heating method adopts furnace heating and gradient heating. First, treat at 33-37℃ for 3.5-4.5h, then heat to 53-57℃, continue to treat for 3.5-4.5h, then heat to 73-77℃ for 3.5-4.5h, and finally heat to 108-112℃ for 15-17h. During the whole process, the heating rate is kept at 1℃ / min. After the heating step is completed, turn off the blast drying oven and cool with the furnace. Take out the sample when it cools to room temperature.

5. The preparation method according to claim 4, characterized in that In step 1, the method for pre-treating the substrate sample is: using sandpaper to polish the surface of the substrate sample to maintain the surface roughness of the sample at 3.0-3.5 μm; The surface of the sample was then wiped with anhydrous ethanol, dried with a hair dryer, weighed using an electronic balance, and set aside for later use.

6. The preparation method according to claim 4, characterized in that In step 3, the epoxy-silicone hybrid resin includes DOWSIL™ 3092 Silicone Resin; and the glycidoxypropyltrimethoxysilane includes 3-aminopropyltrimethoxysilane.

7. The preparation method according to claim 4, characterized in that In step six, the viscosity of the epoxy-silicone hybrid resin precursor solution to be brushed is maintained in a reasonable range, that is, the epoxy-silicone hybrid resin precursor solution to be brushed is brushed on the sample obtained in step five, and the sample is kept in an upright state. At this time, the flow rate of the epoxy-silicone hybrid resin precursor solution to be brushed is 0.1 mm / s.

8. The preparation method according to claim 4, characterized in that In step six, after the epoxy-organosilicon hybrid resin precursor solution is stirred, it is first transferred to a vacuum box for vacuum degassing operation with a vacuum degree of 0.05-0.08 atmospheres and a treatment time of 10-20 minutes.

9. Use of the anti-icing composite coating with a transition layer structure according to any one of claims 1 to 3 on the surface of an engineering component.

10. The use according to claim 9, characterized in that The engineering components include those with irregular surfaces that require anti-icing operations, including wind turbine blades.

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