CN114558764A - Efficient super-hydrophobic surface preparation method - Google Patents
Efficient super-hydrophobic surface preparation method Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/002—Pretreatement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
Abstract
The invention relates to a preparation method of a high-efficiency super-hydrophobic surface, which comprises the following steps: step 10) cleaning the substrate: cleaning the metal substrate; step 20) laser micro-nano processing: placing the cleaned substrate on a sample table of an ultraviolet nanosecond laser processing system, processing a micro-nano structure on the surface of a metal substrate by utilizing a laser beam, and then ultrasonically cleaning the metal substrate in isopropanol for 5-10 minutes; step 30) silicone oil treatment: dripping 15-25 mu L of mixed solution of dimethyl silicone oil and isopropanol on the metal substrate treated in the step 20); step 40) low-temperature heat treatment: heating the metal substrate treated in the step 30) on a heating plate for 5-10 minutes, taking out, ultrasonically cleaning by using isopropanol, and finally drying in nitrogen flow to obtain the super-hydrophobic surface. The method of the invention improves the preparation efficiency, reduces the preparation cost and ensures no toxicity to organisms and environment.
Description
Technical Field
The invention relates to the technical field of material processing engineering, in particular to a preparation method of an efficient super-hydrophobic surface.
Background
Based on the excellent characteristics of self-cleaning, antibiosis, corrosion resistance, drag reduction, anti-icing and the like exhibited by a super-hydrophobic surface, the super-hydrophobic surface has been widely applied to the fields of rail transit, petroleum equipment, aerospace, medical health and the like.
In the prior art, the main methods for preparing the superhydrophobic surface include low surface energy substance coating, self-assembly, polymer imprinting, electrostatic spinning, etching, laser processing and the like. Among them, the laser processing method is widely used due to its advantages of high process flexibility, high degree of automation, low environmental pollution, high preparation accuracy, and the like. However, the preparation efficiency is still a major problem of the laser processing method in the actual industrial production, which is mainly due to the following reasons: 1. most laser surface treatment processes need to use small light spots and repeated scanning for many times, so that the preparation efficiency of laser processing is low; 2. the laser treated surface exhibited superhydrophilic properties. In order to realize the conversion from super-hydrophilic to super-hydrophobic characteristics of the surface, the surface needs to be placed in the air for 3-7 days. Hydrophobic groups in the air are deposited on the surface to realize the super-hydrophobic characteristic, and the preparation period of the super-hydrophobic surface is greatly increased. 3. The conversion of the laser-treated surface from superhydrophilic to superhydrophobic character can be accelerated by some post-treatment processes, however these post-treatment processes also take hours. Meanwhile, some methods such as chemical infiltration methods require fluorine-containing chemical reagents, and the high chemical toxicity of the fluorine-containing chemical reagents also limits the application of the fluorine-containing chemical reagents in the fields of biomedicine and the like.
In summary, it is highly desirable to develop a highly efficient, low-cost and non-toxic superhydrophobic surface preparation process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-efficiency super-hydrophobic surface preparation method to improve the preparation efficiency.
The technical scheme adopted by the invention is as follows:
a method for preparing a high-efficiency super-hydrophobic surface comprises the following steps:
step 10) cleaning the substrate: cleaning the metal substrate;
step 20) laser micro-nano processing: placing the cleaned metal substrate on a sample table of an ultraviolet nanosecond laser processing system, processing a micro-nano structure on the surface of the metal substrate by utilizing a laser beam, and then ultrasonically cleaning the metal substrate in isopropanol for 5-10 minutes;
step 30) silicone oil treatment: dripping a mixed solution of simethicone and isopropanol on the metal substrate treated in the step 20);
step 40) low-temperature heat treatment: heating the metal substrate treated in the step 30) on a heating plate, taking out and ultrasonically cleaning the metal substrate by using isopropanol, and finally blowing the metal substrate in nitrogen flow to obtain the super-hydrophobic surface.
The further technical scheme is as follows:
the metal substrate is AISI304 stainless steel, red copper, brass or Ti-6Al-4V titanium alloy.
In the step 10): and sequentially placing the metal substrate in acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning, and then placing the metal substrate in nitrogen flow for drying.
In the step 10): and ultrasonically cleaning the metal substrate in acetone, absolute ethyl alcohol and deionized water for 10-15 minutes respectively.
In the step 20): the ultraviolet nanosecond laser processing system adopts an ultraviolet nanosecond pulse laser, the wavelength of the laser is 355nm, the pulse width is 10ns, the pulse repetition frequency is 40-60 kHz, the laser power is 5.8-6.5W, the pulse energy is 0.1-0.16 mJ, and the laser power density is 0.23-0.57 GW/cm2The diameter of an effective light spot after focusing is about 60m, the laser scanning speed is 5-50 mm/s, and the scanning area of a laser beam is 10mm multiplied by 10 mm.
In the step 20): the surface structure of the micro-nano structure is a unidirectional, annular or crossed micron-scale groove structure, and submicron-scale or nano-scale sputtering particles are covered on the micron-scale groove structure; the distance between the grooves is 100 to 300 μm, and the depth of the grooves is 15 to 25 μm.
In the step 30), the volume of the dropped mixed solution is 15-25 mu L, the volume fraction of the dimethyl silicone oil in the mixed solution is 0.2-0.4%, and the volume fraction of the isopropanol solution is 99.6-99.8%.
In the step 40), the temperature of the heating plate is 100-150 ℃, and the heating time is 5-10 minutes.
The invention has the following beneficial effects:
the invention greatly shortens the preparation period, improves the preparation efficiency and reduces the preparation cost. And simultaneously, the harmlessness to organisms and the environment is ensured.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention. Wherein: 1. a laser; 2. an attenuator; 3. a beam amplifier; 4. a galvanometer; 5. a cooling system; 6. a controller; 7. a computer; 8. a sample stage; 9. a sample; 10. heating plates; a is silicone oil treatment; b is low-temperature heat treatment; and c, ultrasonic cleaning.
FIG. 2 is a three-dimensional contour test result of the surface after the laser micro-nano processing of the invention.
FIG. 3 is an SEM image of the surface after the laser micro-nano processing of the invention.
FIG. 4 shows EDS spectra of surfaces prepared by different treatment methods. Wherein: (a) is an untreated surface; (b) processing the surface for laser micro-nano processing; (c) the invention adopts a laser-silicone oil-heat treated surface.
Fig. 5 is a contact angle measurement of a drop of water for a surface prepared using different treatments. Wherein: (a) is an untreated surface; (b) processing the surface for laser micro-nano processing; (c) the surface is treated by adding silicone oil after laser micro-nano processing; (d) is a heat-treated surface; (e) adding silicone oil to treat the surface after heat treatment; (f) the invention adopts a laser-silicone oil-heat treated surface.
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
Referring to fig. 1, the method for preparing a highly effective superhydrophobic surface of the present application includes the following steps:
step 10) cleaning the metal substrate: and sequentially placing the metal substrate in acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning, and then placing the metal substrate in nitrogen flow for drying.
Step 20) laser micro-nano processing: placing the cleaned metal substrate on a sample table of an ultraviolet nanosecond laser processing system, processing a micro-nano structure on the surface of the metal substrate by utilizing a laser beam, and then ultrasonically cleaning the metal substrate in isopropanol for 5-10 minutes;
step 30) silicone oil treatment: dripping a mixed solution of simethicone and isopropanol on the metal substrate treated in the step 20);
step 40) low-temperature heat treatment: heating the metal substrate treated in the step 30) on a heating plate, taking out and ultrasonically cleaning the metal substrate by using isopropanol, and finally blowing the metal substrate in nitrogen flow to obtain the super-hydrophobic surface.
The metal substrate is AISI304 stainless steel, red copper, brass or Ti-6Al-4V titanium alloy, etc.
The preparation method mainly comprises two process steps: laser micro-nano processing and post-processing.
The laser processing equipment adopts a TH-UV200A ultraviolet nanosecond laser processing platform produced by Suzhou Tianhong laser company, and the laser is an ultraviolet nanosecond pulse laser AWAVE 355-15W-30K produced by Advanced Optowave company. As shown in FIG. 1, a sample 9 is placed on a sample stage 8, and laser beams are emitted by a laser 1, pass through an attenuator 2 and a beam amplifier 3, enter a galvanometer 4, and are connected with a controller 6 through software of a computer 7 to realize control of laser beam scanning patterns. The galvanometer 4 is connected with a cooling system 5.
Wherein the wavelength of the laser is 355nm, the pulse width is 10ns, the pulse repetition frequency is 40-60 kHz, the laser power is 5.8-6.5W, the pulse energy is 0.1-0.16 mJ, and the laser power density is 0.23-0.57 GW/cm2The diameter of an effective light spot after focusing is about 60 mu m, the laser scanning speed is 5-50 mm/s, and the scanning area of a laser beam is 10mm multiplied by 10 mm.
Specifically, in the silicone oil post-treatment, 15-25 mu L of mixed solution is dripped, the volume fraction of dimethyl silicone oil in the mixed solution is 0.2-0.4%, and the volume fraction of isopropanol solution is 99.6-99.8%. The temperature of the heating plate 10 used for low-temperature heat treatment is 100-150 ℃, and the heating time is 5-10 minutes.
The preparation method of the high-efficiency super-hydrophobic surface is further illustrated by the following specific examples.
Example 1:
and step 10), cutting the red copper substrate into a size of 10mm multiplied by 10mm, then ultrasonically cleaning the red copper substrate for 10 minutes by using acetone, absolute ethyl alcohol and deionized water in sequence to remove pollutants on the surface of the substrate, and then drying the red copper substrate in nitrogen flow.
Step 20) carrying out laser micro-nano processing on the surface, wherein the selected laser parameters are as follows: the pulse width is 10ns, the laser wavelength is 355nm, the pulse repetition frequency is 40kHz, the laser power is 6.5W, the pulse energy is 0.16mJ, and the laser power density is 0.57GW/cm2The effective spot diameter after focusing is about 60 μm, the laser scanning speed is 50mm/s, and the laser beam scanning area is 8mm × 8 mm. The laser-prepared substrate was placed in isopropanol for 5 minutes of ultrasonic cleaning.
Step 30) dripping 15 mu L of mixed solution of dimethyl silicone oil with volume fraction of 0.2% and isopropanol with volume fraction of 99.8% on the metal substrate treated in the step 20).
And step 40) heating the metal substrate treated in the step 30) on a heating plate for 10 minutes, taking out and ultrasonically cleaning the metal substrate by using isopropanol, and finally blowing the metal substrate in a nitrogen flow to obtain the super-hydrophobic surface.
Resting 5 μ L of deionized water on the surface after step 20), the contact angle of the water drop being 0 °, exhibiting superhydrophilic properties; standing 5 μ L of deionized water on the surface after step 40), the contact angle of a water drop is as high as 156.3 degrees, and excellent super-hydrophobic performance is shown.
Example 2:
step 10) cutting a 304 stainless steel substrate into a size of 15mm multiplied by 15mm, then ultrasonically cleaning the substrate for 12 minutes by using acetone, absolute ethyl alcohol and deionized water in sequence to remove pollutants on the surface of the substrate, and then blowing the substrate in a nitrogen flow for drying.
Step 20) carrying out laser micro-nano processing on the surface, wherein the selected laser parameters are as follows: pulse width of 10ns, laser wavelength of 355nm, pulse repetition frequency of 60kHz, laser powerThe optical power is 5.8W, the pulse energy is 0.1mJ, and the laser power density is 0.23GW/cm2The effective spot diameter after focusing is about 60 μm, the laser scanning speed is 20mm/s, and the laser beam scanning area is 12mm × 12 mm. The laser-prepared substrate was placed in isopropanol for ultrasonic cleaning for 10 minutes.
And step 30) dripping 20 mu L of mixed solution of dimethyl silicone oil with volume fraction of 0.4% and isopropanol with volume fraction of 99.6% on the metal substrate treated in the step 20).
And step 40) heating the metal substrate treated in the step 30) on a heating plate for 5 minutes, taking out and ultrasonically cleaning the metal substrate by using isopropanol, and finally blowing the metal substrate in a nitrogen flow to obtain the super-hydrophobic surface.
Standing 5gL of deionized water on the surface after the step 20), wherein the contact angle of a water drop is 0 DEG, and the super-hydrophilic characteristic is shown; standing 5 μ L of deionized water on the surface after step 40), the contact angle of a water drop is as high as 159.2 degrees, and excellent super-hydrophobic performance is shown.
Example 3:
and step 10) cutting the Ti-6Al-4V substrate into a size of 20mm multiplied by 20mm, then ultrasonically cleaning the substrate for 15 minutes by using acetone, absolute ethyl alcohol and deionized water in sequence to remove pollutants on the surface of the substrate, and then blowing the substrate in nitrogen flow for drying.
Step 20) carrying out laser micro-nano processing on the surface, wherein the selected laser parameters are as follows: the pulse width is 10ns, the laser wavelength is 355nm, the pulse repetition frequency is 50kHz, the laser power is 6.1W, the pulse energy is 0.12mJ, and the laser power density is 0.43GW/cm2The effective spot diameter after focusing is about 60 μm, the laser scanning speed is 10mm/s, and the laser beam scanning area is 15mm × 15 mm. The laser-prepared substrate was placed in isopropanol for ultrasonic cleaning for 8 minutes.
Step 30) dripping 25 mu L of mixed solution of dimethyl silicone oil with volume fraction of 0.3% and isopropanol with volume fraction of 99.7% on the metal substrate treated in the step 20).
And step 40) heating the metal substrate treated in the step 30) on a heating plate for 8 minutes, taking out and ultrasonically cleaning the metal substrate by using isopropanol, and finally blowing the metal substrate in a nitrogen flow to obtain the super-hydrophobic surface.
Resting 5 μ L of deionized water on the surface after step 20), the contact angle of the water drop being 0 °, exhibiting superhydrophilic properties; standing 5 μ L of deionized water on the surface after step 40), the contact angle of a water drop is as high as 154.6 degrees, and excellent super-hydrophobic performance is shown.
The technical effects achieved by the preparation method of the present application are analyzed below.
First, in terms of surface structure, as shown in fig. 2, a three-dimensional contour of a surface after laser micro-nano processing according to the present application is shown. As can be seen from fig. 2, the surface exhibits a regularly arranged crossing micro-scale groove structure through the laser micro-nano processing. Scanning of the three-dimensional topography revealed that the grooves had a pitch of about 150 μm and a depth of about 20 μm.
Fig. 3 shows SEM test results of the surface after the laser micro-nano processing in the present application. By observing SEM pictures with different multiples, the boundary of each laser-induced micro-groove is distributed with some submicron and nanometer particles. The particles are mainly formed by the steps of locally heating, vaporizing and ionizing the surface of a material in the interaction process of laser and the material, generating high-pressure plasma expansion and depositing through the ablation of the material and the plasma spraying effect.
The laser micro-nano processing technology can induce the generation of multi-level (micron-submicron-nanometer) micro-nano structures. Compared with a near-infrared nanosecond laser with the wavelength of 1064nm, the ultraviolet laser with the wavelength of 355nm is used, so that the accurate control of the metal surface structure is guaranteed, the heat effect in the laser processing process can be reduced, the heat affected zone is reduced, the high-quality surface multi-level micro-nano structure is prepared, and a foundation is laid for realizing the super-hydrophobic characteristic of the metal surface.
Second, the surface chemical properties are shown in fig. 4, which are the results of the chemical compositions of different surfaces measured by EDS spectroscopy.
Fig. 4(a) is the result of an untreated surface. As can be seen from fig. 4a, Cu, C and O elements can be detected on the untreated surface. Wherein, Cu element is originated from the base material, O element is originated from the oxidation of the surface layer of the base material, and C element is originated from the slight pollution of the surface of the base material. However, the chemical element composition of the laser micro-nano processed surface (shown in fig. 4 (b)) exhibited some variation compared to the untreated surface. The largest variations are due to the C and O elements, except for some variation in the content of the matrix material elements.
Fig. 4(b) shows the result of laser micro-nano processing of the surface. As can be seen from fig. 4b, after the laser micro-nano processing, the content of C element on the surface is obviously reduced, and at the same time, the content of O element is obviously increased, which indicates that the laser micro-nano processing not only induces the generation of the periodic micro-nano structure on the metal surface, but also significantly oxidizes the surface, thereby generating a large amount of hydroxyl (-OH) and carboxyl (-COOH) groups on the surface. For the surface treated by adding silicone oil and heat treatment after the laser micro-nano processing (the laser-silicone oil-heat treatment surface shown in fig. 4 (c)), the chemical components of the surface are significantly changed compared with the surface treated by the laser micro-nano processing.
Fig. 4(c) is the result of laser-silicone oil-heat treatment of the surface employed in the present application. As can be seen from fig. 4c, the chemical changes are mainly the following two aspects: the content of the C element on the laser-silicon oil-heat treatment surface is obviously increased, and the existence of the Si element on the laser-silicon oil-heat treatment surface is detected. The increase of the content of the element C is mainly caused by that the low-temperature heat treatment accelerates the deposition of nonpolar carbon-containing hydrophobic groups (such as-CH 2-, -CH3, C ═ C and other functional groups) in the air on the metal surface. The Si element is derived from a mixed solution of silicone oil and isopropyl alcohol dripped on the surface. In the low-temperature heat treatment process, silicon atoms in the mixed solution are fully deposited on the surface of the metal to form a silicon-containing film. The surface is promoted to generate super-hydrophobic characteristics by means of co-depositing carbon-containing hydrophobic groups with hydrophobic characteristics and a silicon-containing film on the laser-silicone oil-heat treatment surface.
Thirdly, in terms of surface wettability, as shown in fig. 5, contact angle measurement results of the surface to water drops are prepared by using different treatment methods.
Fig. 5(a) is a water droplet contact angle image of an untreated surface, which was measured to have a water droplet contact angle of 82.1 ± 2.5 °, demonstrating that the surface has hydrophilic properties.
Fig. 5(b) is a contact angle image of a water drop on the surface after the laser micro-nano processing treatment, and the measured surface contact angle is reduced to 0 °, which indicates that the metal surface after the laser treatment is in a saturated Wenzel state, so that the surface shows a significant super-hydrophilic characteristic. The reason for analyzing the method mainly comprises the following two points: (1) the micro roughness of the metal surface is obviously increased by laser micro-nano processing treatment, so that the water drop is converted from an unstable Cassie state to a saturated Wenzel state on a laser-induced microstructure composite interface; (2) a large number of hydroxyl groups (-OH) and carboxyl groups (-COOH) generated on the surface are polar groups and have extremely strong hydrophilic characteristics, and the increase of the content of the hydroxyl groups (-OH) and the carboxyl groups (-COOH) also leads to the enhancement of the surface hydrophilicity.
Further, the surface contact angles increased to 76.8 ± 1.8 °, 87.2 ± 1.5 ° and 96.5 ± 1.6 ° respectively by three processes of laser micro-nano machining treatment + silicone oil treatment (fig. 5(c)), heat treatment (fig. 5(d)), and silicone oil + heat treatment (fig. 5(e)) were analyzed. This indicates that both silicone oil treatment and heat treatment can raise the contact angle of the surface to some extent, but then are not sufficient to achieve superhydrophobic properties of the surface.
For the laser-silicone oil-thermal treatment process employed in the present application (fig. 5(f)), the surface contact angle reached 159.2 ± 2.1 °. The laser micro-nano processing treatment, the heat treatment and the silicone oil treatment have equal importance for realizing the super-hydrophobic characteristic. The laser micro-nano processing induces a multi-level micro-nano structure on the surface, and the surface chemistry can be changed by heat treatment and silicone oil treatment, so that the surface energy is reduced. The combined action of the multilevel surface micro-nano structure and the lower surface energy can ensure that the surface realizes the super-hydrophobic characteristic.
In the aspect of preparation efficiency, compared with other super-hydrophobic surface preparation methods, the preparation efficiency is greatly improved.
This is mainly reflected in: (1) the processing methods of coating low-surface-energy substances, self-assembly, polymer imprinting, electrostatic spinning, etching and the like are long in time consumption and expensive in equipment; (2) the laser treated surface exhibited superhydrophilic properties. In order to realize the conversion from super-hydrophilic to super-hydrophobic characteristics of the surface, other laser processing methods need to arrange the surface onThe super-hydrophobic property is realized by depositing hydrophobic groups in the air on the surface after the surface is placed in the air for 3 to 7 days, or the conversion from super-hydrophilicity to the super-hydrophobic property of the laser-treated surface can be accelerated by a post-treatment process for a plurality of hours. (3) The laser surface treatment efficiency is ensured (the scanning speed can reach 1.89cm at most2Min), the post-treatment process of silicone oil treatment is adopted, and the conversion from super-hydrophilic to super-hydrophobic property of the laser treated surface can be completed in only 5-10 minutes, so that the preparation efficiency of the super-hydrophobic surface is greatly improved. Meanwhile, the mixed solution of the silicone oil and the isopropanol used in the application is harmless to organisms and environment, and is expected to be widely applied in various fields.
Claims (8)
1. A preparation method of a high-efficiency super-hydrophobic surface is characterized by comprising the following steps:
step 10) cleaning the substrate: cleaning the metal substrate;
step 20) laser micro-nano processing: placing the cleaned metal substrate on a sample table of an ultraviolet nanosecond laser processing system, processing a micro-nano structure on the surface of the metal substrate by utilizing a laser beam, and then ultrasonically cleaning the metal substrate in isopropanol for 5-10 minutes;
step 30) silicone oil treatment: dripping a mixed solution of dimethyl silicone oil and isopropanol on the metal substrate treated in the step 20);
step 40) low-temperature heat treatment: heating the metal substrate treated in the step 30) on a heating plate, taking out and ultrasonically cleaning the metal substrate by using isopropanol, and finally blowing the metal substrate in nitrogen flow to obtain the super-hydrophobic surface.
2. The method for preparing the high-efficiency superhydrophobic surface according to claim 1, wherein the metal substrate is AISI304 stainless steel, red copper, brass or Ti-6Al-4V titanium alloy.
3. The method for preparing a highly efficient superhydrophobic surface according to claim 1, wherein in the step 10): and sequentially placing the metal substrate in acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning, and then placing the metal substrate in nitrogen flow for drying.
4. The method for preparing a highly efficient superhydrophobic surface according to claim 1 or 3, wherein in the step 10): and ultrasonically cleaning the metal substrate in acetone, absolute ethyl alcohol and deionized water for 10-15 minutes respectively.
5. The method for preparing a highly efficient superhydrophobic surface according to claim 1, wherein in the step 20): the ultraviolet nanosecond laser processing system adopts an ultraviolet nanosecond pulse laser, the wavelength of the laser is 355nm, the pulse width is 10ns, the pulse repetition frequency is 40-60 kHz, the laser power is 5.8-6.5W, the pulse energy is 0.1-0.16 mJ, and the laser power density is 0.23-0.57 GW/cm2The diameter of an effective light spot after focusing is about 60 mu m, the laser scanning speed is 5-50 mm/s, and the scanning area of a laser beam is 10mm multiplied by 10 mm.
6. The method for preparing a highly efficient superhydrophobic surface according to claim 5, wherein in the step 20): the surface structure of the micro-nano structure is a unidirectional, annular or crossed micron-scale groove structure array, and submicron-scale or nano-scale sputtering particles are covered on the micron-scale groove structure; the distance between the grooves is 100 to 300 μm, and the depth of the grooves is 15 to 25 μm.
7. The method for preparing the high-efficiency superhydrophobic surface according to claim 5, wherein in the step 30), the volume of the dropped mixed solution is 15-25 μ L; the volume fraction of the dimethyl silicone oil in the mixed solution is 0.2-0.4%, and the volume fraction of the isopropanol solution is 99.6-99.8%.
8. The preparation method of the high-efficiency superhydrophobic surface according to claim 5, wherein the temperature of the heating plate in the step 40) is 100-150 ℃ and the heating time is 5-10 minutes.
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| CN115595579A (en) * | 2022-10-31 | 2023-01-13 | 中国地质大学（北京）（Cn） | Hydrophobic anti-icing coating on surface of front compression blade of engine and preparation method and application thereof |
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