A method for preparing MXene-based super-slip anti-icing and wear-resistant surface by chemically assisted laser texturing
By chemically assisted laser texturing to prepare Mxene-based super-slip anti-icing and wear-resistant surfaces, the problems of easy structural damage and easy volatilization of lubricants in existing super-slip anti-icing surfaces during mechanical load impact and long-term service are solved, and anti-icing performance with high stability and wear resistance is achieved.
Patent Information
- Application Number
- CN202311211565.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-20
- Publication Date
- 2025-10-03
- Estimated Expiration
- 2043-09-20
AI Technical Summary
When the existing super-slip anti-icing surface is subjected to mechanical load impact or long-term service, the rough structure of the base is easily destroyed and the lubricant is easily volatilized, resulting in a decrease in anti-icing performance and insufficient wear resistance.
Chemical-assisted laser texturing was used to prepare an MXene-based ultra-slip anti-icing and wear-resistant surface. A single layer of MXene was prepared by wet chemical etching, mixed with an adhesive, sprayed, and textured on the surface. It was then modified with a silane coupling agent and chemically grafted with active lubricating oil to form a strong anti-icing and wear-resistant surface.
The prepared super-slip surface has excellent wear resistance, anti-icing and photothermal properties. The surface is strong, the lubricant is highly stable, and it can maintain anti-icing performance after multiple deicing cycles. It has a low friction coefficient and a simple application process.
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Figure CN117181563B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a method for preparing an Mxene-based super-slip anti-icing and wear-resistant surface by chemically assisted laser texturing, and belongs to the technical field of nano anti-icing and wear-resistant coatings. Background Art
[0002] Inspired by the super-slippery properties of the pitcher lip of the Nepenthes plant, researchers have recently fabricated various rough structures through hydrothermal, chemical etching, and sol-gel methods. These structures are then infused with lubricants to create super-slippery surfaces (SLIPS) that mimic the pitcher plant's slippery properties. The lubricant on the SLIPS surface completely isolates the underlying roughness from the air, eliminating pinning points caused by physical structural defects, inhibiting ice nucleation, and preventing tiny droplets from entering the structure and forming ice. This technology holds great promise for applications in liquid-repellent anti-icing applications, such as aircraft wings, power transmission lines, and wind turbines. However, in practical use, SLIPS surfaces still face numerous challenges: 1) The underlying roughness of the superslippery surface is easily damaged by mechanical loads or long-term service, thereby reducing the substrate's service life. 2) The surface oil film directly impacts the SLIPS's liquid repellency and anti-icing properties. When subjected to load impact, exposure to radiation, or fluid erosion, the oil film evaporates or dissolves, causing the oil film to become incomplete. This exposes the underlying roughness, hindering the sliding of liquids across the surface and acting as nucleation sites for ice, weakening the anti-icing capabilities of the sample. To improve the liquid repellency and anti-icing stability of superslippery surfaces, researchers have investigated the effect of the SLIPS substrate's roughness on the stability of the surface oil film. Kim et al. proposed that SLIPS with nanostructured roughness substrates are more effective in resisting shear forces under water erosion, while microstructured and micro-nano composite structures are more susceptible to lubricant loss. To further enhance the substrate's roughness's affinity for lubricants, researchers have pretreated the substrate's roughness. Howell fluorinated the prepared rough structure. After oil drainage, the residual lubricant mass on the fluorinated surface was more than ten times that of the untreated surface. Gaurav et al. constructed SLIPS on a SiO2 porous coating after methylation. After multiple mechanical load stimulations, the structure was destroyed and SLIPS lost its water repellency. In summary, the rough substrate of SLIPS not only needs to meet a certain structural strength to cope with load impact, but also needs to have a high adsorption capacity for lubricants so that the lubricant can be stably combined with the rough substrate. However, the rough structure of the substrate prepared using inorganic materials has good wear resistance and mechanical durability, but weak affinity for lubricants; and the coating prepared from organic materials will swell after the lubricant is injected into the rough structure, resulting in a decrease in mechanical strength.
[0003] Although a large number of super-slip anti-icing surfaces have been designed and applied, in order to achieve long-term service of super-slip anti-icing surfaces, it is still necessary to develop a super-slip anti-icing and wear-resistant surface preparation scheme that has high chemical affinity to lubricants, a rough base structure that is strong and wear-resistant, and still has anti-icing performance after multiple deicing. Summary of the Invention
[0004] This invention aims to develop a method for creating an ultra-slippery, anti-icing, and wear-resistant MXene-based surface through chemically assisted laser texturing. A single layer of MXene is prepared using wet chemical etching, mixed with a binder, and then sprayed onto a metal sheet. Lasers are then used to create a textured structure on the MXene coating, which serves as a reservoir for lubricating oil. The surface is then modified with a silane coupling agent. Finally, active lubricating oil is grafted onto the modified MXene coating through a chemical reaction, resulting in an ultra-slippery, hydrophobic surface with excellent anti-icing and wear-resistant properties. The resulting ultra-slip surface exhibits excellent wear resistance, anti-icing, photothermal, and omniphobic properties, as well as a durable surface and a simple application process.
[0005] The object of the present invention is to provide a method for preparing an Mxene-based super-slip anti-icing and wear-resistant surface by chemically assisted laser texturing.
[0006] In order to achieve the purpose of the present invention, the technical solution adopted is:
[0007] A method for preparing an MXene-based super-slip anti-icing and wear-resistant surface by chemically assisted laser texturing comprises the following steps:
[0008] Step 1: Preparation of single-layer MXene:
[0009] 40 ml of 9 mol / L hydrochloric acid and 3.2 g of LiF were added to a reactor. Deionized water was then added until halfway up the reactor. The mixture was allowed to react at 800 rpm at 40°C for 15 minutes. 2 g of titanium aluminide was slowly added to the reactor in small amounts and stirred for 48 hours. The resulting mixture was then centrifuged at 3500 rpm for 1 minute. 2 mol / L HCl was added to the upper layer and centrifuged again, repeating this process 2-3 times. The mixture was then washed with water several times until the pH was neutral. Maintaining the temperature below 35°C, the resulting solution was purged with nitrogen and then sonicated for one hour. Finally, the product was centrifuged at 3500 rpm for 30 minutes. The upper black solution was the monolayer of MXene.
[0010] Step 2: Preparation of MXene coating:
[0011] The monolayer of MXene from step 1 was ultrasonically dispersed in anhydrous ethanol for 3 minutes, and then an inorganic binder was added and sprayed onto the pretreated metal sheet surface. Finally, the monolayer of MXene was firmly adhered to the substrate surface after oven curing to obtain a MXene coating.
[0012] Step 3: Laser texturing structure of MXene coating surface:
[0013] The Mxene coating of step three is laser textured into a patterned structure to obtain a Mxene coating substrate with a textured patterned structure; the patterned structure includes one or more of a continuous structure and a discrete structure.
[0014] Step 4: Modify the textured MXene coating
[0015] The silane coupling agent is dispersed in anhydrous ethanol, and then the textured MXene coating substrate obtained in step 3 is immersed in the silane coupling agent dispersion and fully reacted for three hours to obtain a laser-textured and modified MXene coating substrate; the silane coupling agent is one or more of a vinyl silane coupling agent, a mercapto silane coupling agent, an epoxy silane coupling agent, and an amino silane coupling agent.
[0016] Step 5: Prepare super-slip anti-icing and wear-resistant surface:
[0017] The laser-textured and silanized MXene coating substrate was immersed in an active lubricant solution, a photoinitiator was added, and the substrate was irradiated under UV light for 1 hour. After being placed vertically for 10 minutes, an ultra-slip, anti-icing, and wear-resistant coating was obtained.
[0018] In one embodiment of the present invention, the volume ratio of the anhydrous ethanol in step 2 to the monolayer MXene is 1%-10%.
[0019] In one embodiment of the present invention, the inorganic binder in step 2 is one or more of phosphate, silicate, and silica sol.
[0020] In one embodiment of the present invention, the metal sheet in step 2 includes one or more of an iron sheet, an aluminum sheet, a magnesium sheet, a copper sheet, and a silver sheet.
[0021] In one embodiment of the present invention, the volume ratio of the inorganic binder in step 2 to anhydrous ethanol is 1%-20%.
[0022] In one embodiment of the present invention, the inorganic binder dispersion in step 2 is added dropwise to the monolayer MXene dispersion, ultrasonicated for 3 minutes, and then continuously stirred before spraying.
[0023] In one embodiment of the present invention, the oven temperature in step 2 is heated at 80-120° C. for 1-6 hours. In one embodiment of the present invention, the pretreatment in step 2 is to use 500, 1000, and 2000 mesh sandpaper to smooth the metal sheet like a mirror, ultrasonicate for 1 minute to remove particles generated during the polishing process, and finally use dilute hydrochloric acid pickling to remove the surface oxide film.
[0024] In one embodiment of the present invention, the post-treatment in step three is plasma bombardment for 0-10 minutes.
[0025] In one embodiment of the present invention, the laser texturing in step three includes one or more of nanosecond laser texturing, picosecond laser texturing, femtosecond laser texturing, and carbon dioxide laser texturing.
[0026] In one embodiment of the present invention, the discrete structure described in step three includes one or more of a circle, a hexagon, a square, a triangle, and a rhombus; the continuous structure includes one or more of a linear groove, a V-shaped groove, a sinusoidal groove, and a grid.
[0027] In one embodiment of the present invention, the laser processing parameters in step 3 are a scanning speed of 50-2000 mm / s, a scanning number of 1-20 times, and a laser power of 0.1-30 W.
[0028] In one embodiment of the present invention, the diameter of the laser textured structure in step three is 10-600 μm, and the pitch is 50-2000 μm.
[0029] In one embodiment of the present invention, the vinyl silane coupling agent described in step 4 includes one or more of vinyltrimethoxysilane, vinyltriethoxysilane, and vinyltrichlorosilane; the mercapto silane coupling agent includes one or more of 3-mercaptopropyltrimethoxysilane and 3-mercaptopropylmethyldimethoxysilane; the epoxy silane coupling agent includes one or more of gamma-glycidylpropylmethyldimethoxysilane and 3-glycidyloxypropylmethyldimethoxysilane; the amino silane coupling agent includes any one or more of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane.
[0030] In one embodiment of the present invention, the volume ratio of the silane coupling agent in step 4 to anhydrous ethanol is 1%-20%.
[0031] In one embodiment of the present invention, the photoinitiator in step five comprises one or more of benzoin, benzoin ethyl ether, and benzoin butyl ether.
[0032] In one embodiment of the present invention, the active lubricant in step five is one or more of amino-terminated perfluoropolyether lubricant, thiol-terminated perfluoropolyether lubricant, epoxy-terminated perfluoropolyether lubricant, and vinyl-terminated perfluoropolyether lubricant.
[0033] In one embodiment of the present invention, the mass ratio of the photoinitiator in step five to the active lubricating oil is 1%-10%.
[0034] Beneficial effects of the present invention:
[0035] (1) The ultra-slippery surface prepared by the present invention has good photothermal properties because the substrate is a black MXene coating. Ice melts rapidly on the surface under light, and sliding on the ultra-slippery surface is possible simply by tilting. This is a passive deicing strategy with great application prospects.
[0036] (2) The present invention uses laser to texture the surface of the MXene coating, which not only provides a storage site for the lubricant, but also increases the surface hardness during the processing, making the structure more stable and firm, and has a significant protective effect on the lubricant stored therein. After multiple anti-icing tests, it still maintains anti-icing performance.
[0037] (3) The MXene coating prepared by the present invention has excellent tribological properties. The laser-textured structure can store the wear debris generated during the friction process, and its wedge-shaped gap can provide fluid dynamic pressure. The prepared ultra-slip surface still maintains a low friction coefficient of 0.02 after 2000 friction cycles, which provides a guarantee for the long-term service of the coating.
[0038] (4) The synergistic effect of laser-textured structure adsorption and storage of lubricants and chemical covalent grafting anchoring greatly improves the stability of the oil film on the super-slippery surface, and it can still maintain liquid repellency after multiple spin coating and deionized water flushing tests. BRIEF DESCRIPTION OF THE DRAWINGS
[0039] Figure 1 The wettability and lyophobicity test characterization of the super-slip, ice-resistant, and wear-resistant surface in Example 1; wherein, (a) is the change in contact angle during the preparation process; (b) is the contact angle and sliding angle of different organic solvents on the super-slip surface; (c) is the sliding conditions of different organic dyeing solvents on the super-slip surface.
[0040] Figure 2 This is a test characterization of the oil film stability performance of the super-slip, anti-icing and wear-resistant surface in Example 1; wherein, (a) is the change in water contact angle of circular pits with different geometric parameters before and after spin coating; (b) is the change in DMSO contact angle of circular pits with different geometric parameters before and after spin coating; (c) is the change in water sliding angle of circular pits with different geometric parameters before and after spin coating; (d) is the change in DMSO sliding angle of circular pits with different geometric parameters before and after spin coating.
[0041] Figure 3 The tribological performance test characterization of the super-slip, anti-icing and wear-resistant surface in Example 1 is shown.
[0042] Figure 4The anti-icing performance test results of the super-slip anti-icing and wear-resistant surface in Example 1 are as follows: (a) shows the ice formation delay of circular dimples with different geometric parameters; (b) shows the ice adhesion strength of circular dimples with different geometric parameters; (c) shows the change in ice adhesion strength of the super-slip anti-icing and wear-resistant surface over multiple deicing cycles; and (d) shows the change in contact angle and sliding angle of the super-slip anti-icing and wear-resistant surface over multiple deicing cycles.
[0043] Figure 5 The hardness and adhesion test characterization of the MXene coating in Example 1.
[0044] Figure 6 This is the circular pit structure in Example 1.
[0045] Figure 7 It is the square columnar junction in Example 5.
[0046] Figure 8 It is the hexagonal columnar structure in Example 6. DETAILED DESCRIPTION
[0047] In order to more clearly understand the technical content of the present invention, the following embodiments are given in detail, the purpose of which is only to better understand the content of the present invention but not to limit the scope of protection of the present invention.
[0048] Examples of what is included in the claims
[0049] Test Method
[0050] Surface morphology observation: The morphology of the particles was observed using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultra-depth of field microscopy.
[0051] Chemical composition testing: X-ray photoelectron spectroscopy (XPS), X-ray energy dispersive spectroscopy (EDS), Raman spectroscopy, and X-ray diffraction (XRD) were used to test the chemical composition of the particles.
[0052] Surface oil film stability testing: The stability of the super-slippery surface oil film was determined by measuring the mass loss of the surface lubricant before and after spin coating and deionized water rinsing. The super-slippery surface was placed on a benchtop glue dispenser (KW-4T, Institute of Microelectronics, Chinese Academy of Sciences) and spun at 600 rpm for 1 minute. The mass loss was measured every 10 seconds. The surface was then rinsed with deionized water (10 cm in height), and the mass loss was measured after each 10 ml of deionized water rinse.
[0053] Lyophobicity Test: Static contact angles and sliding angles of the coatings were measured using a JC2000DM Contact Angle Meter (Shanghai Zhongchen Digital Technology Co., Ltd.). The test liquids were water, DMSO, or other liquids with varying surface tensions. A 10-μl droplet of test liquid was placed onto the coating, and the contact angle was measured. The angle at which the droplet began to slide was determined by varying the sample's tilt on the rotating stage. Each sample was tested five times, and the average and standard deviation were calculated.
[0054] Tribological performance test: Pin-on-disc friction and wear tester (Anton Pear TRB 3 ) to test the friction coefficient of different samples. A 200HVS-5 digital microhardness tester was used to measure the surface hardness of the coating. An ultra-depth-of-field microscope (OLYMPUS DSX1000) was used to observe the surface morphology of the samples after friction, and the wear loss was calculated based on the three-dimensional profile.
[0055] Anti-icing performance testing: A camera monitored and recorded the sample's ice formation time at a -10° angle and ice melting time at a light intensity of 1. The sample's photothermal deicing performance was also measured at a 10° tilt angle. An HP-200 digital push-pull instrument was used to measure the ice binding strength of icicles on the sample surface. The ice adhesion strength and sliding angle were measured over 20 deicing cycles to characterize the anti-icing durability.
[0056] Coating mechanical properties test: According to GB / T 6479-2006 and GB / T 9286-1998 standards, the pencil hardness test and grid scratch test were used to test the hardness and bonding strength of the MXene coating.
[0057] Example 1
[0058] A method for preparing an iron sheet having an ultra-slip, anti-icing and wear-resistant surface comprises the following steps:
[0059] 40 ml of 9 mol / L hydrochloric acid and 3.2 g of LiF were added to a reactor. Deionized water was then added to the reactor halfway up the reactor. The mixture was allowed to react at 800 rpm at 40°C for 15 minutes. 2 g of titanium aluminide was weighed and slowly added to the reactor, stirring for 48 hours. The resulting mixture was then centrifuged at 3500 rpm for 1 minute. 2 mol / L HCl was added to the upper layer and centrifuged again, repeating this process 2-3 times. The mixture was then washed with water several times until the pH was neutral. Maintaining the temperature below 35°C, the resulting solution was purged with nitrogen and ultrasonicated for one hour. Finally, the product was centrifuged at 3500 rpm for 30 minutes. The upper black solution was the monolayer of MXene. The monolayer of MXene was ultrasonically dispersed in anhydrous ethanol for 3 minutes. Phosphate was then added to the monolayer of MXene dispersion and sprayed onto the surface of a pretreated iron sheet. Finally, after oven curing, the monolayer of MXene firmly adhered to the substrate surface, resulting in a MXene coating. Nanosecond laser was used to texture circular pits on the surface of MXene coating. Figure 6 As shown, circular pits with diameters of 50-150 microns and spacings of 50-200 microns, designated T1-T9, were formed to produce a MXene-coated substrate with circular pits. The coating surface was then post-treated. Vinyltrimethoxysilane was dispersed in anhydrous ethanol, and the textured MXene-coated substrate was then immersed in the vinyltrimethoxysilane dispersion for three hours to fully react, resulting in a silanized MXene-coated substrate with circular pits. The laser-textured and silanized MXene-coated substrate was then immersed in a mercapto-terminated perfluoropolyether lubricant. Benzoin ethyl ether was dissolved in n-hexane and then added to the mercapto-terminated perfluoropolyether lubricant. The substrate was then irradiated under UV light for 1 hour. After being placed vertically for 10 minutes, an ultra-slip, anti-icing, and wear-resistant surface was obtained.
[0060] The obtained iron sheet with super-slip anti-icing and wear-resistant surface was subjected to performance tests, and the test results of its liquid repellency, oil film stability, tribological properties, anti-icing performance and coating mechanical properties are shown in the following table. Figure 1 、 Figure 2 、 Figure 3 、 Figure 4 and Figure 5 shown.
[0061] from Figure 1 It can be seen that the contact angle does not change much during the process of preparing the super-slip anti-icing and wear-resistant surface by the original iron sheet, spraying the MXene coating, laser texturing the coating, silanization of the textured surface, and finally pouring perfluoropolyether lubricant, and most organic solvents with low surface energy can slide on the super-slip anti-icing and wear-resistant surface, indicating that the successful grafting of vinyl-terminated perfluoropolyether lubricant on the surface gives the textured MXene coating surface excellent liquid repellency.
[0062] from Figure 2It can be seen that only the contact angle and sliding angle of T1 and T2 changed greatly before and after spin coating, showing poor surface oil film stability. Therefore, the diameter of the pits of T1 and T2 is small, and the number of hydroxyl groups in the pits after plasma bombardment is less than that of T3-T9, and the reaction with vinyltrimethoxysilane is less. In addition, the texture spacing of T1-T2 is small, and the number of pits on the entire sample surface is more, and the amount of oil stored in the pits is also more. After spin coating, perfluoropolyether lubricant is more easily lost from the pits, thus showing poor surface oil film stability. The contact angle and sliding angle of T3-T9 did not change much before and after the spin coating test, among which T3 changed the least, showing the best oil film stability, indicating that the synergistic strategy of texture pits with appropriate diameter and spacing and chemical covalent grafting improves the stability of the super-slip, anti-icing and wear-resistant surface oil film.
[0063] from Figure 3 It can be seen that compared with the original iron sheet, thanks to the low shear strength and high specific surface area of MXene, the MXene coating has an extremely low friction coefficient of only 0.13 under dry friction. Because nanosecond lasers are long-pulsed lasers with a large heat-affected zone, burrs and bumps inevitably appear around the processed area, which is equivalent to increasing the surface roughness. Therefore, the friction coefficient of the MXene coating increases after laser texturing. The ultra-slip anti-icing and wear-resistant surface prepared by the present invention has a lyophilic nature. When the oil film inevitably loses or breaks during the friction process, its lyophilic nature can promote the formation of the oil film. The laser-textured pits provide a wedge-shaped gap, forming hydrodynamic lubrication. Some MXene will be peeled off during the friction process, and the friction coefficient gradually decreases as the MXene peels off. The peeled MXene acts as an additive to the liquid lubricant and participates in the friction process to reduce the friction coefficient. After 2000 friction cycles, it still maintains a low friction coefficient of 0.02. This shows that the ultra-slip anti-icing and wear-resistant surface prepared by the present invention has good tribological properties.
[0064] from Figure 4 It can be seen that the super-slip anti-icing and wear-resistant surfaces of T1-T9 all exhibit low ice adhesion strength and long icing delay, and the changing trend of their anti-icing performance is the same as the surface oil film stability test results. In the anti-icing durability test, the ice adhesion strength, contact angle and sliding angle of the super-slip anti-icing and wear-resistant surface prepared by the present invention within 20 deicing cycles change very little, indicating that the solid Mxene coating provides a stable base roughness structure for the super-slip anti-icing and wear-resistant surface, and the synergistic effect of the laser texturing physical structure and the chemical covalent grafting strategy enables the perfluoropolyether lubricant to be stably present on the surface, showing excellent anti-icing durability.
[0065] from Figure 5The hardness and bonding strength of the MXene coating were tested using a pencil hardness test and a cross-hatch scratch test according to GB / T 6479-2006 and GB / T 9286-1998 standards. The test results show that the MXene coating's hardness reached 5H and its adhesion reached 1-degree. This indicates that the phosphate binder and high-temperature curing firmly secure the single-layer MXene to the substrate surface, resulting in excellent mechanical properties.
[0066] Example 2:
[0067] A method for preparing a magnesium sheet having an ultra-slip, anti-icing, and wear-resistant surface comprises the following steps:
[0068] The preparation process for MXene was the same as in Example 1. Silica sol was then added to a monolayer of MXene dispersion and sprayed onto the pretreated magnesium sheet surface. Finally, after oven curing, the monolayer of MXene firmly adhered to the magnesium sheet surface, resulting in an MXene coating. The MXene coating was textured using a picosecond laser to create circular pits with a diameter of 50-150 microns and a spacing of 50-200 microns, yielding an MXene-coated substrate with circular pits. The coating surface was then post-treated. 3-Mercaptopropyltrimethoxysilane was dispersed in anhydrous ethanol. The textured MXene-coated substrate was then immersed in the 3-Mercaptopropyltrimethoxysilane dispersion and allowed to react for three hours, resulting in a silanized MXene-coated substrate with circular pits. The laser-textured and silanized MXene-coated substrate was then immersed in a vinyl-terminated perfluoropolyether lubricant. Butyl benzoin ether was dissolved in n-hexane, then the vinyl-terminated perfluoropolyether lubricant solution was added and irradiated under UV light for 1 hour. After being placed vertically for 10 minutes, an ultra-slip, anti-icing and wear-resistant surface was obtained.
[0069] Example 3:
[0070] A method for preparing an aluminum sheet having an ultra-slip, anti-icing, and wear-resistant surface comprises the following steps:
[0071] The preparation process of Mxene is the same as that of Example 1. Subsequently, silicate is added to a monolayer Mxene dispersion and sprayed onto the surface of the pretreated aluminum sheet. Finally, after oven curing, the monolayer Mxene firmly adheres to the surface of the aluminum sheet to obtain a Mxene coating. The Mxene coating is textured using a femtosecond laser to give circular pits with a diameter of 50-150 microns and a spacing of 50-200 microns, thereby obtaining a Mxene coating substrate with circular pits. The coating surface is then post-treated. 3-glycidyloxypropylmethyldimethoxysilane is dispersed in anhydrous ethanol, and the textured Mxene coating substrate is then immersed in a 3-glycidyloxypropylmethyldimethoxysilane dispersion and allowed to react for three hours to obtain a silanized Mxene coating substrate with circular pits. The laser-textured and silanized MXene-coated substrate was immersed in an amino-terminated perfluoropolyether lubricant. Benzoin was fully dissolved in n-hexane and then added to the amino-terminated perfluoropolyether lubricant. The substrate was then irradiated under UV light for one hour. After standing vertically for 10 minutes, an ultra-slip, anti-icing, and wear-resistant surface was obtained.
[0072] Example 4:
[0073] A method for preparing an aluminum sheet having an ultra-slip, anti-icing, and wear-resistant surface comprises the following steps:
[0074] The preparation process for MXene is the same as in Example 1. Silicate is then added to a monolayer MXene dispersion and sprayed onto the pretreated aluminum sheet. Finally, after oven curing, the monolayer MXene firmly adheres to the aluminum sheet, resulting in a MXene coating. The MXene coating is textured using a femtosecond laser to create circular pits with a diameter of 50-150 microns and a spacing of 50-200 microns, yielding an MXene-coated substrate with circular pits. The coating surface is then post-treated. 3-Aminopropyltriethoxysilane is dispersed in anhydrous ethanol, and the textured MXene-coated substrate is then immersed in the 3-aminopropyltriethoxysilane dispersion and allowed to react for three hours, resulting in a silanized MXene-coated substrate with circular pits. The laser-textured and silanized MXene-coated substrate is then immersed in an epoxy-terminated perfluoropolyether lubricant. Benzoin is fully dissolved in n-hexane, then added to the epoxy-terminated perfluoropolyether lubricant and irradiated under UV light for 1 hour. After being placed vertically for 10 minutes, an ultra-slip, anti-icing and wear-resistant surface was obtained.
[0075] Example 5:
[0076] The other preparation processes are consistent with Example 1. Picosecond laser is used to texture square columnar structures on the surface of the Mxene coating, with a side length of 50-200 microns and a spacing of 50-300 microns. Figure 7 As shown, a MXene coating substrate with a square columnar structure is obtained, and the coating surface is post-treated.
[0077] Example 6:
[0078] The other preparation processes were consistent with those in Example 1. Picosecond laser was used to texture the surface of the Mxene coating with a hexagonal columnar structure with a side length of 50-500 μm and a spacing of 50-300 μm. Figure 8 As shown, a MXene coating substrate with a hexagonal columnar structure is obtained, and the coating surface is post-treated.
Claims
1. A method for preparing an ultra-slip, anti-icing and wear-resistant surface, characterized in that: The steps include: Step 1: Preparation of monolayer MXene: Hydrochloric acid and lithium fluoride were added to a reactor, stirred at 40°C, and titanium aluminide was added and stirred for 48 hours. The resulting mixed solution was then centrifuged several times, acid-washed, and washed with water until the pH was neutral. The resulting solution was purged with nitrogen for one hour. Finally, the product was centrifuged, and the upper black solution was the monolayer MXene; Step 2: Preparation of an inorganic adhesive composite MXene coating: The single-layer MXene obtained in step 1 is dispersed in anhydrous ethanol, and then an inorganic adhesive is added and sprayed on the surface of the pretreated metal sheet. Finally, after oven curing, the single-layer MXene is firmly adhered to the surface of the substrate to obtain the MXene coating; Step 3: Laser texturing a patterned structure on the surface of the MXene coating: laser texturing the patterned structure of the MXene coating in step 3 to obtain a MXene coating substrate with a textured patterned structure; the patterned structure includes one or more of a continuous structure and a discrete structure; Step 4: chemically modifying the textured MXene coating, dispersing the silane coupling agent in anhydrous ethanol, and then immersing the textured patterned structure MXene coating substrate obtained in step 4 into the silane coupling agent dispersion to obtain a modified textured MXene coating substrate; the silane coupling agent is one or more of a vinyl silane coupling agent, a mercapto silane coupling agent, an epoxy silane coupling agent, and an amino silane coupling agent; Step 5: Prepare a super-slip anti-icing and wear-resistant surface: Immerse the textured and modified sample in an active lubricating oil solution, add a photoinitiator and irradiate it under ultraviolet light, and place it vertically for 10 minutes to obtain a super-slip anti-icing and wear-resistant coating.
2. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The volume ratio of the inorganic binder to Mxene in step 2 is 1:2-1:10; the inorganic binder is one or more of phosphate, silicate, and silica sol; and the curing temperature is 80-120° C. and heated for 1-6 hours.
3. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The laser texturing in step three includes one or more of nanosecond laser texturing, picosecond laser texturing, femtosecond laser texturing, and carbon dioxide laser texturing.
4. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The discrete structure described in step three includes one or more of a circle, a hexagon, a square, a triangle, and a rhombus; the continuous structure includes one or more of a linear groove, a V-shaped groove, a sinusoidal groove, and a grid; the diameter of the laser textured pattern is 10-600 mm and the spacing is 50-2000 mm.
5. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The processing parameters of the laser texturing in step 3 are scanning speed 50-2000 mm / s, scanning times 1-20 times, and laser power 0.1-30 W.
6. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The vinyl silane coupling agent described in step 4 includes one or more of vinyltrimethoxysilane, vinyltriethoxysilane, and vinyltrichlorosilane; the mercapto silane coupling agent includes one or more of 3-mercaptopropyltrimethoxysilane and 3-mercaptopropylmethyldimethoxysilane; the epoxy silane coupling agent includes one or more of gamma-glycidylpropylmethyldimethoxysilane and 3-glycidyloxypropylmethyldimethoxysilane; the amino silane coupling agent includes any one or more of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane.
7. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The photoinitiator in step five includes one or more of benzoin, benzoin ethyl ether, and benzoin butyl ether.
8. The method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1, characterized in that: The active lubricant described in step five includes one or more of amino-terminated perfluoropolyether lubricant, mercapto-terminated perfluoropolyether lubricant, epoxy-terminated perfluoropolyether lubricant, and vinyl-terminated perfluoropolyether lubricant.
9. Application of the method for preparing a super-slip anti-icing and wear-resistant surface according to claim 1 in the fields of liquid repellency, extending freezing time, reducing ice adhesion strength, reducing friction and wear, and long-term service of the coating.