CN115716928B - Preparation method of super-amphiphobic surface with inclined stepped mushroom head micro-column structure - Google Patents
Preparation method of super-amphiphobic surface with inclined stepped mushroom head micro-column structure Download PDFInfo
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- CN115716928B CN115716928B CN202211465581.7A CN202211465581A CN115716928B CN 115716928 B CN115716928 B CN 115716928B CN 202211465581 A CN202211465581 A CN 202211465581A CN 115716928 B CN115716928 B CN 115716928B
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Abstract
The invention discloses a preparation method of a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure, which comprises the following steps of: continuously drawing a two-dimensional circle on the surface of a polyethylene terephthalate adhesive tape/contracted polystyrene board double-layer film by using femtosecond laser, separating the polyethylene terephthalate adhesive tape/polystyrene board double-layer film from a matrix of an x-y plane in the two-dimensional circle under the cutting action of the laser to form mushroom head microcolumns, and scanning semicircles at the bottom of the grown mushroom head microcolumn structure by using the femtosecond laser due to different laser scanning times among different rows to form an inclined stepped mushroom head microcolumn structure; finally, carrying out fluorosilane modification on the sample and spraying SO 2 fluoroPOS a suspension. The inclined stepped mushroom head micro-column structure prepared by the invention has excellent repellency to low surface tension liquid, and can realize directional bouncing of low surface energy mixed liquid drops.
Description
Technical Field
The invention belongs to the technical field of super-amphiphobic functional materials, and particularly relates to a preparation method of a super-amphiphobic surface with an inclined stepped mushroom head microcolumn structure.
Background
The impact of droplets on solid surfaces is a very common phenomenon in natural and industrial applications, and proper utilization of droplets can solve many biological, environmental and health problems. Such as self-cleaning, antibacterial, pesticide spraying, anti-icing, and heat transfer. Bacterial surface colonization has become an important issue in hospitals and the food industry, and bacterial adhesion and aggregation often lead to serious health and hygiene consequences. The orientation and rapid transport of the droplets in the bouncing state can reduce the available contact area between bacteria and the surface, reducing the extent of bacterial retention.
Among them, superhydrophobic surfaces (SHSs) are considered as excellent candidates for antibacterial materials. These SHSs have good bacterial liquid repellency. It was observed that the droplets could bounce on these surfaces; however, unless the SHSs deviate from horizontal, the droplets eventually settle on these surfaces after bouncing. Over time, the air layer trapped on the superhydrophobic surface eventually becomes depleted, the superhydrophobic surface vanishes, allowing bacteria to grow on the surface. In contrast to the symmetrical SHSs antimicrobial strategy, the asymmetrical SHSs allow the droplets to bounce directionally and quickly off the surface. Various strategies have been proposed to achieve directional bouncing. Significant progress has been made in the directional bouncing of water droplets, but the directional bouncing of composite liquids and other liquids with lower surface tension remains a major challenge. In nature, these droplets are mostly present in the form of composite droplets. Composite droplets have important applications in targeted drug delivery, food industry, waste water management and microfluidics. Thus, it is crucial to understand the diffusion, splashing and directional rebound behavior of composite droplets. To address these problems, it is desirable to design a new structure that can direct the rebound of the composite drop to a preferred area.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a method for preparing a super-amphiphobic surface having a sloped stepped mushroom head micropillar structure, comprising the steps of:
step one, inducing mushroom head micro-pillars to self-grow on the surface of a material by utilizing laser to obtain a stepped mushroom head micro-pillar structure array;
step two, utilizing laser to induce the step mushroom head microcolumn to incline in situ, and obtaining an inclined step mushroom head microcolumn structure on the surface of the material;
step three, soaking a material with an inclined stepped mushroom head micro-column structure on the surface in a prepared fluorosilane solution, drying, and fluorinating the surface of the material with the inclined stepped mushroom head micro-column structure;
step four, SO is configured 2 Spraying SO on the surface of the fluorinated inclined stepped mushroom head micro-column structure by using a spray gun on the fluoroPOS suspension 2 And @ fluoroPOS suspension to obtain the super-amphiphobic surface with the inclined stepped mushroom head micro-column structure.
Preferably, in the first step, the method for processing the inclined stepped mushroom head micro-column structure includes: continuously drawing a preprogrammed two-dimensional circle on the surface of the polyethylene terephthalate adhesive tape/polystyrene board double-layer film by using femtosecond laser, wherein every two rows of two-dimensional circles are a group, the two-dimensional circles are separated from the polyethylene terephthalate adhesive tape/polystyrene board double-layer film substrate on an x-y plane by ablation, and as the number of times of laser scanning circles is increased, the heat accumulated by the laser causes the shrinkage growth of a bottom polystyrene board layer, but the high-temperature-resistant polyethylene terephthalate adhesive tape layer on the top layer is not changed, so that a stepped mushroom head microcolumn is formed;
in the second step, the specific method for inducing the stepped mushroom head microcolumns to incline by using laser in situ comprises the following steps: and scanning the semicircle at one side part of the bottom of the grown mushroom head microcolumn by using the femtosecond laser again to form an inclined stepped mushroom head microcolumn structure.
Preferably, in the third step, the fluorosilane solution is a mixed solution of absolute ethyl alcohol and 1H, 2H-perfluoro-dialkyltriethoxysilane, wherein the mass ratio of 1H, 2H-perfluoro-dialkyltriethoxysilane to absolute ethyl alcohol is 1:80.
Preferably, the scanning times of the first femtosecond laser to each group of two-dimensional circles are increased in a range of 40-65, and the scanning times of the second femtosecond laser to each group of two-dimensional circles are 10-15; the power of the two femtosecond lasers is 90mW, and the scanning speed is 50mm/s.
Preferably, in the first step, the material is a polyethylene terephthalate tape/polystyrene board double-layer film structure, the bottom layer is a contracted polystyrene board, and the top layer is a polyethylene terephthalate tape.
Preferably, in the third step, the soaking time of the inclined stepped mushroom head micro-column structure in the prepared fluorosilane solution is 12 hours, the drying temperature is 80 ℃, and the drying time is 2 hours.
Preferably, in the fourth step, SO 2 The preparation method of the @ fluoroPOS suspension comprises the following steps: dispersing silicon dioxide in absolute ethyl alcohol and ammonia water solution, rapidly adding perfluoro silane and ethyl orthosilicate under intense stirring after ultrasonic treatment, reacting for a certain time at room temperature to form uniform SO 2 fluoroP OS suspension; wherein the mass volume ratio of the silicon dioxide, the absolute ethyl alcohol, the ammonia water, the perfluoro silane and the ethyl orthosilicate is 0.2g:44mL:6mL:120 muL:30 muL.
Preferably, the ultrasonic treatment time of the silicon dioxide in the anhydrous ethanol and ammonia water solution is 30min, the stirring speed is 600r/min, and the room temperature reaction time is 2h.
Preferably, in the fourth step, the distance between the spray gun and the inclined stepped mushroom head micro-column structure surface is 10cm.
Preferably, the polyethylene terephthalate tape on top of the polyethylene terephthalate tape/polystyrene board bilayer film has a thickness of 10 μm.
The invention at least comprises the following beneficial effects:
firstly, the method prepares the heavy micro-column by the self-growth induced by the laser on the surface of the double-layer film of the polyethylene terephthalate adhesive tape/polystyrene board, wherein the growth speed is 317+/-14 mu m/s, which is 3 orders of magnitude higher than that of the traditional photo-regulating monomer polymerization method;
secondly, the invention can reduce the rebound time of the liquid drop and can lead the liquid drop to rebound towards the preferred area in a directional way;
thirdly, after fluorination and spraying, the inclined stepped mushroom head micro-column structure shows excellent repellency to low-surface tension liquid;
fourth, by taking advantage of the flexibility of polystyrene boards, their super-amphiphobicity can be easily transferred to curved surfaces, showing a promising trans-disciplinary potential.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic view of a laser processing of a stepped mushroom head micro-pillar structure of example 1;
FIG. 2 is a tilted view prepared in example 1 SEM photograph of stepped mushroom head micropillar structure;
FIG. 3 is a schematic diagram showing the bouncing of water droplets on the surface of an inclined stepped mushroom head micro-pillar structure;
FIG. 4 is a schematic diagram showing the bouncing of 30% ethanol on the surface of the inclined stepped mushroom head micropillar structure prepared in example 1.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
As shown in fig. 1, the present embodiment provides a method for preparing a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure, comprising the following steps:
step one, processing an inclined stepped mushroom head micro-column structure on the surface of a polyethylene terephthalate (PET) adhesive tape/Polystyrene (PS) plate double-layer film material, wherein the specific method comprises the following steps: continuously drawing a preprogrammed two-dimensional circle on the surface of a polyethylene terephthalate (PET) adhesive tape/Polystyrene (PS) plate double-layer film by using femtosecond laser, wherein the scanning times of each two-dimensional circle are increased in a range of 45-65 per two rows of one group, namely, in 20 groups of two-dimensional circles, the scanning times of the first group of two-dimensional circles are 45 times, the scanning times of each two-dimensional circle are increased in sequence with 1 as an arithmetic difference, the PET/PS double-layer film in the two-dimensional circles is separated from a matrix on an x-y plane (namely, the plane of the PET/PS double-layer film outside the two-dimensional circles) through ablation, the heat accumulated by laser causes the PS plate at the bottom layer to shrink and grow along with the increase of the times of the laser scanning circles, but the high-temperature resistant PET adhesive tape at the top layer can not change, so that a stepped mushroom head microcolumn is formed; scanning semicircle at one side part of the bottom of the grown mushroom head microcolumn by using femtosecond laser again, wherein the scanning times of each group of two-dimensional circles are 15, so that an inclined stepped mushroom head microcolumn structure is formed, and an SEM (scanning electron microscope) picture of the inclined stepped mushroom head microcolumn structure is shown in figure 2; the power of the two times of femtosecond laser is 90mW, and the scanning speed is 50mm/s;
step two, soaking the processed sample in a prepared fluorosilane solution for 12 hours for modification, and then placing the modified fluorosilane solution in an oven at 80 ℃ for 2 hours, wherein the fluorosilane solution comprises absolute ethyl alcohol and 1H, 2H and 2H-perfluoro dialkyl triethoxysilane, and the mass ratio of the perfluoro silane to the absolute ethyl alcohol is 1:80;
step three, SO is configured 2 The @ fluoroPOS suspension, spraying SO on the surface of the dried inclined stepped mushroom head microcolumn structure by using a spray gun 2 Forming a fluorine-silicon coating on the surface of the inclined stepped mushroom head micro-column structure by virtue of a fluoroPOS suspension, wherein the distance between a spray gun and the surface of the inclined stepped mushroom head micro-column structure is 10cm; SO (SO) 2 The preparation steps of the @ fluoroPOS suspension are as follows: dispersing 0.2g of silicon dioxide in a solution containing 44mL of absolute ethyl alcohol and 6mL of ammonia water solution, carrying out ultrasonic treatment for 30min, rapidly adding 120 mu L of perfluorosilane and 30 mu L of tetraethoxysilane under intense stirring at 600r/min, and reacting for 2h at room temperature to form uniform SO 2 fluoroPOS suspension.
The contact angle of water drops on the surface of the inclined stepped mushroom head micro-column structure in the example 1 is 160 degrees, and the rolling angle is 1 degree; as shown in fig. 3, the water drop bounces by 5.99mm in the direction of the inclined stepped mushroom head microcolumn structure surface prepared in the embodiment, and the rolling distance is 2.4mm; as shown in FIG. 4, 30% ethanol was directed to bounce at a distance of 2cm on the surface of the inclined stepped mushroom structure prepared in this example.
Example 2
The embodiment provides a preparation method of a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure, which comprises the following steps:
step one, processing an inclined stepped mushroom head micro-column structure on the surface of a polyethylene terephthalate (PET) adhesive tape/Polystyrene (PS) plate double-layer film material, wherein the specific method comprises the following steps of: continuously drawing a preprogrammed two-dimensional circle on the surface of a polyethylene terephthalate (PET) adhesive tape/Polystyrene (PS) plate double-layer film by using femtosecond laser, wherein the scanning times of each two-dimensional circle are increased in a range of 40-60 per two rows of one group, namely, in 20 groups of two-dimensional circles, the scanning times of the first group of two-dimensional circles are 40 times, the scanning times of each two-dimensional circle are increased in sequence with 1 as an arithmetic difference, the PET/PS double-layer film in the two-dimensional circles is separated from a matrix on an x-y plane (namely, the plane of the PET/PS double-layer film outside the two-dimensional circles) through ablation, the heat accumulated by laser causes the PS plate at the bottom layer to shrink and grow along with the increase of the times of the laser scanning circles, but the high-temperature resistant PET adhesive tape at the top layer can not change, so that a stepped mushroom head microcolumn is formed; scanning semicircle at one side of the bottom of the grown mushroom head microcolumn by using femtosecond laser again, wherein the scanning times of each group of two-dimensional circles are 15, so that an inclined stepped mushroom head microcolumn structure is formed; the power of the two times of femtosecond laser is 90mW, and the scanning speed is 50mm/s;
step two, soaking the processed sample in a prepared fluorosilane solution for 12 hours for modification, and then placing the modified fluorosilane solution in an oven at 80 ℃ for 2 hours, wherein the fluorosilane solution comprises absolute ethyl alcohol and 1H, 2H and 2H-perfluoro dialkyl triethoxysilane, and the mass ratio of the perfluoro silane to the absolute ethyl alcohol is 1:80;
step three, SO is configured 2 Spraying SO on the surface of the dried inclined stepped mushroom head micro-column structure by using a spray gun on the fluoroPOS suspension 2 Forming a fluorine-silicon coating on the surface of the inclined stepped mushroom head micro-column structure by virtue of a fluoroPOS suspension, wherein the distance between a spray gun and the surface of the inclined stepped mushroom head micro-column structure is 10cm; SO (SO) 2 The preparation steps of the @ fluoroPOS suspension are as follows: will 0.2g of twoDispersing silicon oxide in a solution containing 44mL of absolute ethyl alcohol and 6mL of ammonia water solution, carrying out ultrasonic treatment for 30min, rapidly adding 120 mu L of perfluorosilane and 30 mu L of tetraethoxysilane under the intense stirring of 600r/min, and reacting for 2h at room temperature to form uniform SO 2 fluoroPOS suspension.
The contact angle of the inclined stepped mushroom head microcolumn structure surface in example 2 was measured to be 158 °, the rolling angle was measured to be 2 °, and the directional bouncing distance of 30% ethanol was measured to be 1.7cm.
Example 3
The embodiment provides a preparation method of a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure, comprises the following steps
Step one, processing an inclined stepped mushroom head micro-column structure on the surface of a polyethylene terephthalate (PET) adhesive tape/Polystyrene (PS) plate double-layer film material, the specific method comprises the following steps: continuously drawing a preprogrammed two-dimensional circle on the surface of a polyethylene terephthalate (PET) adhesive tape/Polystyrene (PS) plate double-layer film by using femtosecond laser, wherein the scanning times of each two-dimensional circle are increased in a range of 45-65 per two rows of one group, namely, in 20 groups of two-dimensional circles, the scanning times of the first group of two-dimensional circles are 45 times, the scanning times of each two-dimensional circle are increased in sequence with 1 as an arithmetic difference, the PET/PS double-layer film in the two-dimensional circles is separated from a matrix on an x-y plane (namely, the plane of the PET/PS double-layer film outside the two-dimensional circles) through ablation, the heat accumulated by laser causes the PS plate at the bottom layer to shrink and grow along with the increase of the times of the laser scanning circles, but the high-temperature resistant PET adhesive tape at the top layer can not change, so that a stepped mushroom head microcolumn is formed; scanning semicircle at one side of the bottom of the grown mushroom head microcolumn by using femtosecond laser again, wherein the scanning times of each group of two-dimensional circles are 10, so that an inclined stepped mushroom head microcolumn structure is formed; the power of the two times of femtosecond laser is 90mW, and the scanning speed is 50mm/s;
step two, soaking the processed sample in a prepared fluorosilane solution for 12 hours for modification, and then placing the modified fluorosilane solution in an oven at 80 ℃ for 2 hours, wherein the fluorosilane solution comprises absolute ethyl alcohol and 1H, 2H and 2H-perfluoro dialkyl triethoxysilane, and the mass ratio of the perfluoro silane to the absolute ethyl alcohol is 1:80;
step three, SO is configured 2 The @ fluoroPOS suspension, spraying SO on the surface of the dried inclined stepped mushroom head microcolumn structure by using a spray gun 2 Forming a fluorine-silicon coating on the surface of the inclined stepped mushroom head micro-column structure by virtue of a fluoroPOS suspension, wherein the distance between a spray gun and the surface of the inclined stepped mushroom head micro-column structure is 10cm; SO (SO) 2 The preparation steps of the @ fluoroPOS suspension are as follows: dispersing 0.2g of silicon dioxide in a solution containing 44mL of absolute ethyl alcohol and 6mL of ammonia water solution, carrying out ultrasonic treatment for 30min, rapidly adding 120 mu L of perfluorosilane and 30 mu L of tetraethoxysilane under intense stirring at 600r/min, and reacting for 2h at room temperature to form uniform SO 2 fluoroPOS suspension.
The contact angle of the inclined stepped mushroom head microcolumn structure surface in example 3 was measured to be 157 °, the rolling angle was 3 °, and the directional bouncing distance of 30% ethanol was 1.5cm.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (9)
1. The preparation method of the super-amphiphobic surface with the inclined stepped mushroom head micro-column structure is characterized by comprising the following steps of:
step one, inducing mushroom head micro-pillars to self-grow on the surface of a material by utilizing laser to obtain a stepped mushroom head micro-pillar structure array;
step two, utilizing laser to induce the step mushroom head microcolumn to incline in situ, and obtaining an inclined step mushroom head microcolumn structure on the surface of the material;
step three, soaking a material with an inclined stepped mushroom head micro-column structure on the surface in a prepared fluorosilane solution, drying, and fluorinating the surface of the material with the inclined stepped mushroom head micro-column structure;
step four, SO is configured 2 Spraying SO on the surface of the fluorinated inclined stepped mushroom head micro-column structure by using a spray gun on the fluoroPOS suspension 2 Obtaining super-amphiphobic surface with inclined stepped mushroom head micro-column structure by @ fluoroPOS suspension;
in the first step, the material is a polyethylene terephthalate adhesive tape/polystyrene board double-layer film structure, the bottom layer is a contracted polystyrene board, and the top layer is a polyethylene terephthalate adhesive tape;
SO 2 the preparation method of the @ fluoroPOS suspension comprises the following steps: dispersing silicon dioxide in absolute ethyl alcohol and ammonia water solution, rapidly adding perfluoro silane and ethyl orthosilicate under intense stirring after ultrasonic treatment, reacting for a certain time at room temperature to form uniform SO 2 fluoroPOS suspension.
2. The method for preparing a super-amphiphobic surface with sloped stepped mushroom head micropillar structure according to claim 1, wherein in the first step, the method for processing the sloped stepped mushroom head micropillar structure comprises: continuously drawing a preprogrammed two-dimensional circle on the surface of the polyethylene terephthalate adhesive tape/polystyrene board double-layer film by using femtosecond laser, wherein every two rows of two-dimensional circles are a group, the two-dimensional circles are separated from the polyethylene terephthalate adhesive tape/polystyrene board double-layer film substrate on an x-y plane by ablation, and as the number of times of laser scanning circles is increased, the heat accumulated by the laser causes the shrinkage growth of a bottom polystyrene board layer, but the high-temperature-resistant polyethylene terephthalate adhesive tape layer on the top layer is not changed, so that a stepped mushroom head microcolumn is formed;
in the second step, the specific method for inducing the stepped mushroom head microcolumns to incline by using laser in situ comprises the following steps: and scanning the semicircle at one side part of the bottom of the grown mushroom head microcolumn by using the femtosecond laser again to form an inclined stepped mushroom head microcolumn structure.
3. The method for preparing a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure according to claim 1, wherein in the third step, the fluorosilane solution is a mixed solution of absolute ethyl alcohol and 1H, 2H-perfluoro dialkyl triethoxysilane, wherein the mass ratio of 1H, 2H-perfluoro dialkyl triethoxysilane to absolute ethyl alcohol is 1:80.
4. The method for preparing the super-amphiphobic surface with the inclined stepped mushroom head micro-column structure according to claim 2, wherein the scanning times of the first femtosecond laser on each group of two-dimensional circles are increased in a range of 40-65, and the scanning times of the second femtosecond laser on each group of two-dimensional circles are 10-15; the power of the two femtosecond lasers is 90mW, and the scanning speed is 50mm/s.
5. The method for preparing a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure according to claim 1, wherein in the third step, the soaking time of the inclined stepped mushroom head micro-column structure in the prepared fluorosilane solution is 12h, the drying temperature is 80 ℃, and the drying time is 2h.
6. The method for preparing a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure according to claim 1, wherein in the fourth step, the mass-volume ratio of silicon dioxide, absolute ethyl alcohol, ammonia water, perfluoro silane and ethyl orthosilicate is 0.2g:44mL:6mL:120 μL:30 μL.
7. The method for preparing a super-amphiphobic surface with an inclined stepped mushroom head micro-column structure according to claim 6, wherein the ultrasonic treatment time of silicon dioxide in absolute ethyl alcohol and ammonia water solution is 30min, the stirring speed is 600r/min, and the room temperature reaction time is 2h.
8. The method for preparing a super-amphiphobic surface with inclined stepped mushroom head micro-pillar structures according to claim 1, wherein in the fourth step, a distance between a spray gun and the inclined stepped mushroom head micro-pillar structure surface is 10cm.
9. The method for preparing a super-amphiphobic surface with a sloped stepped mushroom head micropillar structure according to claim 2, wherein the thickness of the polyethylene terephthalate tape on top of the polyethylene terephthalate tape/polystyrene board bilayer film is 10 μm.
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| CN114378460A (en) * | 2022-01-14 | 2022-04-22 | 合肥工业大学 | Bionic hydrophobic micro-column array structure, preparation method thereof and liquid drop control method |
| CN114408856A (en) * | 2022-01-19 | 2022-04-29 | 合肥工业大学 | Inclined micro-column array structure, preparation device and method thereof, and function control method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114378460A (en) * | 2022-01-14 | 2022-04-22 | 合肥工业大学 | Bionic hydrophobic micro-column array structure, preparation method thereof and liquid drop control method |
| CN114408856A (en) * | 2022-01-19 | 2022-04-29 | 合肥工业大学 | Inclined micro-column array structure, preparation device and method thereof, and function control method |
Non-Patent Citations (2)
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| Femtosecond Laser Regulated Ultrafast Growth of Mushroom-Like Architecture for Oil Repellency and Manipulation;Yi Yang et al.;Nano Letters;第21卷;9301-9309 * |
| 基于二氧化硅纳米粒子的抗冲击超双疏涂层的制备及其性能研究;董拴涛;合成材料老化与应用;第49卷(第3期);30-34 * |
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