CN111330829B - Silicon substrate super-hydrophobic surface and preparation method and application thereof - Google Patents
Silicon substrate super-hydrophobic surface and preparation method and application thereof Download PDFInfo
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- CN111330829B CN111330829B CN202010159931.1A CN202010159931A CN111330829B CN 111330829 B CN111330829 B CN 111330829B CN 202010159931 A CN202010159931 A CN 202010159931A CN 111330829 B CN111330829 B CN 111330829B
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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
- B05D7/24—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 for applying particular liquids or other fluent materials
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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
- B05D1/00—Processes for applying liquids or other fluent materials
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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
- 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
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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
- B23K26/0006—Working by laser beam, e.g. welding, cutting or boring taking account of the properties of the material involved
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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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- 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
- B05D2202/00—Metallic substrate
- B05D2202/20—Metallic substrate based on light metals
- B05D2202/25—Metallic substrate based on light metals based on Al
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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
- B05D2203/00—Other substrates
- B05D2203/30—Other inorganic substrates, e.g. ceramics, silicon
Abstract
The invention provides a substrate super-hydrophobic surface and a preparation method and application thereof. The method comprises the steps of firstly treating the surface of a substrate submerged in water by adopting focused femtosecond laser to form a surface periodic nanostructure with deep sub-wavelength order of magnitude parallel to the polarization direction of the laser, thus obtaining a super-hydrophilic surface with large area and uniform distribution, then drying the super-hydrophilic surface, and then treating the super-hydrophilic surface by adopting polydimethylsiloxane to convert the super-hydrophilic surface into super-hydrophobic surface, wherein the obtained super-hydrophobic surface of the substrate can be applied to the fields of water prevention, fog prevention, drag reduction, self-cleaning, micro-fluidic, oil-water separation, fog collection and the like. The PDMS heat treatment technology adopted by the invention has the advantages of safe and nontoxic raw materials, simple operation, short treatment time, material saving, no need of special supporting facilities and low professional requirements on operators.
Description
Technical Field
The invention relates to the crossing field of optical, electrical, computer and material science integration, in particular to a substrate super-hydrophobic surface and a preparation method and application thereof.
Background
The surface wettability (or wettability) of a material is largely determined by both the surface chemical composition and the microscopic geometry of the material. The method comprises two ways of preparing the super-hydrophobic surface, wherein one way is to construct a rough micro-nano structure on the surface of a hydrophobic material, and the other way is to modify the rough surface with a substance with low surface energy so as to reduce the surface free energy. When the material surface forms a micro-nano structure, a contact state model of a liquid drop and the solid surface is changed, the Young state of an ideal smooth solid surface is changed into a Wenzel state or Cassie/Baxter state of a rough solid surface, and the surface wettability of the material is correspondingly changed. Changing the surface chemical composition of a material can change the surface energy of the material, the lower the surface energy, the more hydrophobic the surface of the material. Common ways to construct a superhydrophobic surface are coating, spraying, templating, photolithography, self-assembly, electrochemical, chemical etching, plasma etching, and the like. Common surface modification methods include vapor deposition (a method in which chemical gas or vapor reacts on the surface of a substrate to synthesize a coating or a nanomaterial), chemical grafting (a method in which a reactive group on the surface of a material chemically reacts with a monomer or a macromolecular chain to be grafted to graft the surface), and the like. Common low surface energy reagents capable of realizing surface modification are fluorosilane (fluoroalkyl silane) and Perhydropolysilazane (PHPS), etc., and commonly used for fluorosilane are 1H, 2H-Perfluorodecyltriethoxysilane (1H, 2H-Perfluorodecyltrimethoxysilane, PFDTES) and 1H, 2H-Perfluorodecyltrimethoxysilane (1H, 2H-Perfluorodecyltrimethoxysilane), etc., and these reagents are relatively complicated in purchase and use flow, relatively poor in chemical inertness, expensive in price, toxic in fluorosilane, require special equipment, and are relatively expensive and have high professional requirements on operators.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a substrate super-hydrophobic surface and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
in a first aspect, the present invention provides a method for preparing a superhydrophobic surface of a substrate, comprising the steps of:
(1) inducing a surface periodic nano structure parallel to the polarization direction of laser with deep sub-wavelength order on the surface of a substrate by adopting focused femtosecond laser so as to obtain a super-hydrophilic surface, wherein the substrate is submerged in water, and the surface periodic nano structure is also provided with nano protrusions;
(2) drying the super-hydrophilic surface, and then treating the super-hydrophilic surface by Polydimethylsiloxane (PDMS) to form a polydimethylsiloxane membrane on the super-hydrophilic surface, so as to obtain the super-hydrophobic surface of the substrate;
wherein the substrate is made of silicon.
Sub-wavelength order means that the ratio of the period of the nano-stripe structure to the wavelength of the incident laser is between 0.4 and 1 and does not include 0.4, while deep sub-wavelength order means that the ratio of the period of the nano-stripe structure to the wavelength of the incident laser is 0.4 or less. The preparation method comprises the steps of firstly inducing the surface of a substrate in water to form a surface periodic nano structure parallel to the laser polarization direction by a femtosecond laser micro-nano processing technology, wherein the structure is completely different from a structure (a surface periodic structure vertical to the laser polarization direction in the order of sub-wavelength) formed by inducing the substrate in air by a common femtosecond laser micro-nano processing technology, so that the artificial regulation and control of the distribution of the nano structure can be realized by the method; and then, treating the obtained super-hydrophilic surface by adopting PDMS (polydimethylsiloxane), and realizing the modification of the substrate surface on the basis of not changing the surface nano-structure morphology, so that the super-hydrophilic surface is converted into super-hydrophobic surface.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the femtosecond laser employs a laser having an output center wavelength of 800nm, a pulse width of 100fs, a repetition frequency of 1kHz, is focused by a lens, and the substrate surface is located 5mm below a focal plane of the lens, the laser scanning speed is 0.8mm/s, the laser power is 5.85mW, the laser scanning pitch is 9 μm, and the liquid level height on the substrate surface is 4.5-9.5 mm. When the height of the liquid level on the substrate surface is in the range of 4.5-9.5mm, the influence of the height of the liquid level on the substrate surface on the surface structure is small.
As a preferred embodiment of the preparation method of the present invention, the contact angle of the superhydrophilic surface with water in air is 0-5 deg.
In a preferred embodiment of the preparation method of the present invention, the method of treating with polydimethylsiloxane comprises: placing the super-hydrophilic surface above a polydimethylsiloxane solution, enabling the super-hydrophilic surface to face the polydimethylsiloxane solution, heating and evaporating the polydimethylsiloxane solution, and then cooling to form a polydimethylsiloxane membrane on the super-hydrophilic surface, wherein the polydimethylsiloxane solution comprises a curing agent. Different from the common fluorosilane, the PDMS adopted by the invention is non-toxic, has good chemical inertness, simple using method and low cost; compared with the common soaking method, vapor deposition method, grafting method and the like, the PDMS heat treatment method adopted by the invention is simple, the modification time is short, materials with larger area can be modified, the modification efficiency is high, other special equipment is not needed, the professional requirement on operators is not high, the applicability is strong, and various materials can be modified, including but not limited to silicon, ceramics and aluminum alloy.
As a preferable embodiment of the preparation method, the polydimethylsiloxane solution is mainly prepared from polydimethylsiloxane and a curing agent according to the weight ratio of 10: 1.
As a preferred embodiment of the preparation method, the heating procedure of the heating evaporation is that the temperature is raised from room temperature to 300 ℃ within 5min, and then the temperature is kept at 300 ℃ for 30-90 min.
As a preferred embodiment of the preparation method of the invention, the contact angle of the substrate superhydrophobic surface with water in air is above 150 degrees.
In a second aspect, the invention provides a substrate super-hydrophobic surface prepared by the preparation method.
In a third aspect, the invention provides an application of the substrate superhydrophobic surface, and particularly relates to an application of the substrate superhydrophobic surface in the fields of water prevention, fog prevention, drag reduction, self-cleaning, microfluidics, oil-water separation or fog-water collection.
Compared with the prior art, the invention has the following advantages and beneficial effects: according to the invention, a femtosecond laser micro-nano processing technology is firstly utilized to induce a surface periodic nano structure with a deep sub-wavelength order of magnitude parallel to the polarization direction of laser on the surface to obtain a large-area uniformly distributed super-hydrophilic surface appearance, and then a PDMS heat treatment technology is adopted to modify the super-hydrophilic surface, so that the used raw material PDMS is safe and non-toxic, and compared with the traditional methods such as a soaking method, a vapor deposition method and a grafting method, the PDMS heat treatment technology is simpler, the processing time is shorter, the material is saved, special supporting facilities are not needed, and the professional requirement on an operator is not high; the obtained substrate super-hydrophobic surface can be applied to the fields of water prevention, fog prevention, drag reduction, self-cleaning, micro-fluidic, oil-water separation, fog-water collection and the like.
Drawings
FIG. 1 is a schematic diagram of experimental PDMS heat treatment technology;
FIG. 2 is an SEM (scanning Electron microscope) image of a superhydrophilic surface obtained by inducing a silicon surface with a femtosecond laser;
FIG. 3 is a photograph showing the contact angle of a silicon substrate with water in air, wherein (a) is a superhydrophobic surface of a silicon substrate prepared in comparative example 1, and (b) is a superhydrophobic surface of a silicon substrate prepared in example 1;
FIG. 4 is a photograph of the contact angle of the super-hydrophobic surface of the silicon substrate prepared in example 2 with water in the air;
fig. 5 is a photograph of a contact angle of the superhydrophobic surface of the silicon substrate prepared in comparative example 2 with water in air.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
This example is an example of a method for preparing a superhydrophobic surface of a substrate according to the invention, the method comprising the steps of:
(1) treating the surface of a silicon wafer (the silicon wafer is a substrate) by adopting focused femtosecond laser, wherein the silicon wafer is submerged in water, the thickness of the silicon wafer is 0.5mm, the water depth is 5mm, the output center wavelength of an adopted amplification level laser (manufacturer: American Coherent company, model: Legend) is 800nm, the pulse width is 100fs, the repetition frequency is 1kHz, the femtosecond laser is focused by a lens with the focal length of 15cm, the surface of the silicon wafer to be treated is positioned 5mm below the focal plane of the lens, the laser scanning speed is 0.8mm/s, the laser power is 5.85mW, the laser scanning interval is 9 mu m, and the ultra-hydrophilic surface is obtained after the femtosecond laser treatment;
(2) drying the silicon slice treated in the step (1), and then modifying by adopting a PDMS heat treatment technology, wherein the method comprises the following specific steps: preparing a polydimethylsiloxane solution (prepared by SYLGARD 184 of Dow Corning company, specifically, uniformly mixing a prepolymer (A solution) and a curing agent (B solution) according to a weight ratio of 10: 1), paving the solution on a glass flat plate, placing a silicon wafer above the polydimethylsiloxane solution according to a diagram shown in figure 1, enabling the super-hydrophilic surface of the silicon wafer to face the polydimethylsiloxane solution, then placing the combination in a muffle furnace, raising the temperature from room temperature to 300 ℃ within 5min, then preserving the temperature at 300 ℃ for 90min, cooling to room temperature, and taking out to obtain the silicon substrate super-hydrophobic surface.
The super-hydrophilic surface obtained in the embodiment is characterized by using a scanning electron microscope (manufacturer: czech Thermo Fisher, model: Apreo), and the specific result is shown in fig. 2, so that the silicon wafer surface forms periodic structure distribution parallel to the laser polarization direction with deep sub-wavelength order, the period is about 160nm and is accompanied with nano protrusions, and the periodic structure distribution is completely different from the surface periodic structure perpendicular to the laser polarization with sub-wavelength order in the air; the superhydrophilic surface was measured to have a contact angle with water in air of about 0 °.
The hydrophilicity and hydrophobicity of the superhydrophobic surface of the silicon substrate obtained in this example were characterized by using a fully automatic contact angle measuring instrument (manufacturer: Dataphysics, germany, model: OCA20), and the specific results are shown in fig. 3(b), and the contact angle of the superhydrophobic surface with water in air was measured to be about 150 °.
Example 2
The embodiment relates to a preparation method of a substrate super-hydrophobic surface, which is used for carrying out heat preservation on a silicon wafer for 30 minutes at 300 ℃ when PDMS (polydimethylsiloxane) heat treatment is carried out on the silicon wafer, and comprises the following steps:
(1) obtaining a superhydrophilic surface as in step (1) of example 1;
(2) and (2) airing the silicon wafer treated in the step (1), placing the silicon wafer above a polydimethylsiloxane solution (the same as in the embodiment 1), paving the polydimethylsiloxane solution (the same as in the embodiment 1) on a glass flat plate, placing the combination in a muffle furnace, raising the temperature from room temperature to 300 ℃ within 5min, then preserving the temperature at 300 ℃ for 30min, cooling to room temperature, and taking out to obtain the silicon substrate super-hydrophobic surface. The hydrophilicity and hydrophobicity of the superhydrophobic surface of the silicon substrate obtained in the embodiment are characterized by using a full-automatic contact angle measuring instrument (manufacturer: Dataphysics, germany, model: OCA20), and the specific result is shown in fig. 4, and the contact angle of the superhydrophobic surface and water in the air is about 150 °.
Comparative example 1
The comparative example relates to a preparation method of a substrate super-hydrophobic surface, which is characterized in that a silicon wafer is not subjected to femtosecond laser treatment, but is directly subjected to PDMS heat treatment, specifically, the silicon wafer is placed above a polydimethylsiloxane solution (same as in example 1), wherein the polydimethylsiloxane solution is laid on a glass plate, then the combination is placed in a muffle furnace, the temperature is increased from room temperature (about 23 ℃) to 300 ℃ within 5min, then the temperature is kept at 300 ℃ for 90min, the temperature is reduced to room temperature, and the silicon substrate super-hydrophobic surface is obtained after the combination is taken out. The hydrophilicity and hydrophobicity of the superhydrophobic surface of the silicon substrate obtained in the comparative example were characterized by using a fully automatic contact angle measuring instrument (manufacturer: Dataphysics, germany, model: OCA20), and the specific results are shown in fig. 3(a), and the contact angle of the superhydrophobic surface with water in air was measured to be about 84 °.
Comparative example 2
The comparative example relates to a preparation method of a silicon substrate super-hydrophobic surface, which comprises the following steps:
(1) obtaining a super-hydrophilic surface in the same manner as in the step (1) of example 1;
(2) and (2) drying the super-hydrophilic surface obtained in the step (1), and then modifying by adopting a PDMS spin coating technology to obtain the super-hydrophobic surface of the silicon substrate. The contact angle between the silicon substrate super-hydrophobic surface obtained in the comparative example and water in the air is shown in fig. 5, and the comparison between fig. 5 and fig. 3(b) shows that the contact angle between the silicon substrate super-hydrophobic surface obtained by adopting the PDMS spin coating technology and water in the air is far smaller than the contact angle between the silicon substrate super-hydrophobic surface obtained by adopting PDMS heat treatment and water in the air.
It should be finally noted that the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A preparation method of a substrate super-hydrophobic surface is characterized by comprising the following steps:
(1) inducing a surface periodic nano structure parallel to the polarization direction of laser with deep sub-wavelength order on the surface of a substrate by adopting focused femtosecond laser so as to obtain a super-hydrophilic surface, wherein the substrate is submerged in water, and the surface periodic nano structure is also provided with nano protrusions; in the step (1), the output center wavelength of a laser adopted by the femtosecond laser is 800nm, the pulse width is 100fs, the repetition frequency is 1kHz, the femtosecond laser is focused by a lens, the surface of the substrate is located 5mm below the focal plane of the lens, the laser scanning speed is 0.8mm/s, the laser power is 5.85mW, the laser scanning interval is 9 μm, and the height of the liquid level on the surface of the substrate is 4.5-9.5 mm;
(2) drying the super-hydrophilic surface and then treating the super-hydrophilic surface by adopting polydimethylsiloxane to form a polydimethylsiloxane membrane on the super-hydrophilic surface, namely obtaining the super-hydrophobic surface of the substrate; wherein the substrate is made of silicon; the method for treating by adopting the polydimethylsiloxane comprises the following steps: placing the superhydrophilic surface over a polydimethylsiloxane solution and with the superhydrophilic surface facing the polydimethylsiloxane solution, heating the polydimethylsiloxane solution to evaporate, and then cooling to form a polydimethylsiloxane membrane on the superhydrophilic surface, wherein the polydimethylsiloxane solution comprises a curing agent; the heating procedure of heating evaporation is from room temperature to 300 ℃ within 5min, and then the temperature is kept at 300 ℃ for 30-90 min.
2. The method of claim 1, wherein the superhydrophilic surface has a contact angle with water in air of 0-5 °.
3. The method of claim 1, wherein the polydimethylsiloxane solution is prepared from polydimethylsiloxane and a curing agent in a weight ratio of 10: 1.
4. The method of claim 1, wherein the superhydrophobic surface of the substrate has a contact angle with water in air of 150 ° or more.
5. A superhydrophobic surface of a substrate prepared by the method of any of claims 1-4.
6. The use of the substrate superhydrophobic surface of claim 5, wherein the use is in the field of waterproofing, anti-fogging, drag reduction, self-cleaning, microfluidics, oil-water separation, or mist-water collection.
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| CN113668141B (en) * | 2021-08-25 | 2023-07-04 | 青岛大学 | Preparation method of super-hydrophilic and lipophilic fibrous membrane for kitchen |
| CN114558764A (en) * | 2022-02-11 | 2022-05-31 | 东南大学 | Efficient super-hydrophobic surface preparation method |
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| CN105108342B (en) * | 2015-09-18 | 2017-03-22 | 南开大学 | Method for preparing two-dimensional metallic photonic crystal structure in large area through femtosecond laser direct writing |
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