CN115338542B - Monocrystalline silicon with hydrophobic functional surface and preparation method and application thereof - Google Patents
Monocrystalline silicon with hydrophobic functional surface and preparation method and application thereof Download PDFInfo
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 51
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 230000000737 periodic effect Effects 0.000 claims abstract description 24
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 claims abstract description 8
- 238000002444 silanisation Methods 0.000 claims abstract description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 4
- 239000002086 nanomaterial Substances 0.000 claims abstract description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 238000002679 ablation Methods 0.000 claims description 11
- 238000003754 machining Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- QTRSWYWKHYAKEO-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(1,1,2,2,2-pentafluoroethoxy)silane Chemical group FC(F)(F)C(F)(F)O[Si](OC(F)(F)C(F)(F)F)(OC(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F QTRSWYWKHYAKEO-UHFFFAOYSA-N 0.000 claims description 5
- 230000001939 inductive effect Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000004377 microelectronic Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000002352 surface water Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 3
- 238000005459 micromachining Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003075 superhydrophobic effect Effects 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
-
- 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
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
- B23K26/062—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam
- B23K26/0622—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses
- B23K26/0624—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses using ultrashort pulses, i.e. pulses of 1ns or less
-
- 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
- B23K26/14—Working by laser beam, e.g. welding, cutting or boring using a fluid stream, e.g. a jet of gas, in conjunction with the laser beam; Nozzles therefor
- B23K26/146—Working by laser beam, e.g. welding, cutting or boring using a fluid stream, e.g. a jet of gas, in conjunction with the laser beam; Nozzles therefor the fluid stream containing a liquid
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- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- Laser Beam Processing (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of laser micromachining, and relates to monocrystalline silicon with a hydrophobic functional surface, and a preparation method and application thereof. The preparation method comprises the steps of carrying out laser-assisted water jet processing on the surface of monocrystalline silicon to form a micron-sized structure array on the surface of monocrystalline silicon; forming a nano structure on the surface of the micron-sized structure array by using a femtosecond laser to induce a low-frequency periodic surface structure, thereby forming a micro-nano double-scale layered structure on the surface of monocrystalline silicon; immersing monocrystalline silicon with a micro-nano double-scale layered structure on the surface into hydrophobic silane for silanization treatment, thus obtaining the silicon nitride; in the laser-assisted water jet processing, the water jet is placed in the laser along the scanning speed direction. The invention can make the monocrystalline silicon surface possess hydrophobicity or superhydrophobicity on the basis of forming a micro-nano double-scale layered structure on the monocrystalline silicon surface.
Description
Technical Field
The invention belongs to the technical field of laser micromachining, and relates to monocrystalline silicon with a hydrophobic functional surface, and a preparation method and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Wettability is an important physical property when people study the contact of a solid surface and liquid, and a monocrystalline silicon surface with good hydrophobicity has important application in various fields such as photoelectricity, microelectronics, biomedicine and the like, for example, water drops roll on the surface of a silicon-based solar cell with good hydrophobicity to take away pollutants such as dust accumulated on the surface, so that the surface of the solar cell has self-cleaning property, and the light absorptivity of the cell is improved; in a microelectromechanical system (MEMS), having an excellent hydrophobic silicon-based surface microstructure can effectively reduce adhesion (stiction) while increasing surface roughness, contributing to improved yield and lifetime.
In order to realize the function of hydrophobic self-cleaning on the surface of the material, methods adopted in the prior art include a vapor deposition method, a sol-gel method, a hydrothermal synthesis method, an electrostatic spinning method and the like. However, these methods are limited in application due to the use of large amounts of chemical, or are too costly to be applied on a large scale due to the complicated steps. The laser processing technology has the advantages of arbitrary and controllable processing structure, realization of programming and large-area processing, and environmental friendliness. The laser and the material generally act in a thermal mode, so that the recast layer, the heat affected zone and the like are seriously damaged, and a hydrophobic structure is difficult to form on the surface of the material.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide monocrystalline silicon with a hydrophobic functional surface, and a preparation method and application thereof, and the monocrystalline silicon surface can be made to have hydrophobicity or superhydrophobicity on the basis of forming a micro-nano double-scale layered structure on the monocrystalline silicon surface.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
on one hand, the preparation method of monocrystalline silicon with a hydrophobic functional surface comprises the steps of carrying out laser-assisted water jet processing on the surface of the monocrystalline silicon to form a micron-sized structure array on the surface of the monocrystalline silicon; forming a nano structure on the surface of the micron-sized structure array by using a femtosecond laser to induce a low-frequency periodic surface structure, thereby forming a micro-nano double-scale layered structure on the surface of monocrystalline silicon; immersing monocrystalline silicon with a micro-nano double-scale layered structure on the surface into hydrophobic silane for silanization treatment, thus obtaining the silicon nitride; in the laser-assisted water jet processing, the water jet is placed in the laser along the scanning speed direction.
In the laser-assisted water jet processing, the water jet is placed in the laser along the scanning speed direction, the area of monocrystalline silicon to be processed is heated and softened by the laser and then sheared and removed by the water jet in a plastic mode, so that a recast layer and a heat affected zone generated by laser processing are greatly reduced. Then, the micron-sized surface structure can be rapidly prepared by a laser-assisted water jet processing technology, and on the basis of the micron-sized structure, the low-frequency periodic surface structure is induced by femtosecond laser, so that the functional surface of the layered structure with micro-nano double dimensions is rapidly and controllably constructed on the surface of the array of the micron-sized structure. Finally, after further treatment by hydrophobic silane, the surface of the monocrystalline silicon can be rendered hydrophobic, even super-hydrophobic.
On the other hand, a single crystal silicon having a hydrophobic functional surface is obtained by the above production method.
In a third aspect, use of monocrystalline silicon with a hydrophobic functional surface in the photovoltaic, microelectronics and/or biomedical fields.
The beneficial effects of the invention are as follows:
The invention adopts the method of laser-assisted water jet processing to overcome the serious processing damage problems of the traditional laser texturing surface recast layer, thermal cracking and the like, and simultaneously solves the problem of low femtosecond laser removal efficiency through the processing of laser-assisted water jet processing and femtosecond laser-induced low-frequency periodic surface structure, and can quickly and controllably construct the layered structure functional surface with micro-nano double scale on the monocrystalline silicon surface, and finally the monocrystalline silicon surface has hydrophobicity or superhydrophobicity through further processing of hydrophobic silane.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
Fig. 1 is a schematic diagram of a processing flow of a micro-nano double-scale monocrystalline silicon hydrophobic functional surface prepared by combining laser-assisted water jet with femtosecond laser in an embodiment of the invention, (a) a monocrystalline silicon wafer to be processed, (b) a matrix structure prepared by laser-assisted water jet processing schematic diagram (c) a matrix and V-shaped groove array laser-assisted water jet scanning path (d) laser-assisted water jet, and (e) a micro-nano double-scale structural surface prepared by femtosecond laser processing schematic diagram (f) femtosecond laser processing;
Fig. 2 is a laser scanning microscope image of a micrometer-scale structure array obtained by laser-assisted water jet processing in the embodiment of the present invention, (a) a micrometer-scale matrix structure of embodiment 1, (b) a micrometer-scale V-shaped groove array of embodiment 2, and (c) a micrometer-scale V-shaped groove array of embodiment 3;
FIG. 3 is a scanning electron microscope image of the surface of the micro-nano double-scale matrix structure prepared in example 1 of the present invention;
FIG. 4 is a scanning electron microscope image of the surface of the micro-nano double-scale V-shaped groove array structure prepared in the embodiment 2 of the invention;
fig. 5 is a scanning electron microscope image of the surface of the micro-nano double-scale V-shaped groove array structure prepared in example 3 of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
In view of the problems that the conventional laser texturing surface recast layer, thermal cracking and the like are seriously damaged and the femtosecond laser removal efficiency is low, the micro-nano double-scale hydrophobic functional surface cannot be manufactured on the surface of monocrystalline silicon, and the invention provides monocrystalline silicon with the hydrophobic functional surface, and a preparation method and application thereof.
According to an exemplary embodiment of the invention, a preparation method of monocrystalline silicon with a hydrophobic functional surface is provided, and laser-assisted water jet processing is performed on the monocrystalline silicon surface, so that a micron-sized structure array is formed on the monocrystalline silicon surface; forming a nano structure on the surface of the micron-sized structure array by using a femtosecond laser to induce a low-frequency periodic surface structure, thereby forming a micro-nano double-scale layered structure on the surface of monocrystalline silicon; immersing monocrystalline silicon with a micro-nano double-scale layered structure on the surface into hydrophobic silane for silanization treatment, thus obtaining the silicon nitride; in the laser-assisted water jet processing, the water jet is placed in the laser along the scanning speed direction.
Firstly, processing a micron-sized structure array on the surface of monocrystalline silicon by utilizing a laser-assisted water jet technology. The micron-sized matrix structure can be obtained by scanning the laser-assisted water jet processing device along mutually perpendicular directions, or the micron-sized array structure can be obtained by scanning the laser-assisted water jet processing device along a certain direction in parallel. The laser assisted water jet processing technology can controllably adjust the depth, width and spacing of micro grooves in the micro-scale structure array by adjusting the laser power, pulse width, pulse repetition frequency, water jet pressure, jet offset distance, water jet nozzle target distance, water jet impact angle, scanning speed, scanning spacing and other technological parameters of laser.
Then, a low-frequency periodic surface structure is induced around an ablation threshold by using a femtosecond laser on the surface of the obtained array of micro-scale structures. The center wavelength of the femtosecond laser is 800nm, the pulse width is 35fs, the repetition frequency is 1kHz, and the adjustable technological parameters comprise energy density, defocus (the objective lens is positive and negative away from the surface of the monocrystalline silicon to be processed), scanning speed and direction and the like. By controlling the above-described process parameters, the morphology of the periodic surface structure generated on the surface of the microstructure can be adjusted.
The femtosecond laser is Gaussian beam, and the distribution of the laser intensity along the radial direction r and the propagation direction z is shown in the formulas (1) to (2).
Where I is the laser intensity, z is the length at the beam waist in the direction of beam propagation, r is the length at the radial distance from the center of the spot, P is the beam power, λ is the laser wavelength, and ω 0 is the beam waist radius.
As is known from equations (1) and (2), the laser intensity of the gaussian beam is maximum at the beam waist (i.e., z=0), and decreases as z increases, i.e., the laser intensity gradually decreases as the defocus amount increases positively or negatively.
The results of the study show that near the ablation threshold, a periodic structure of the laser-induced surface appears on the surface of the material. When the femtosecond laser is used for scanning the surface of the micron-sized structure with the energy density near the ablation threshold, the laser intensity of the femtosecond laser injected into the surface of the micron-sized structure can be changed in a gradient way along with the different depths of different positions of the micron-sized structure, and sub-wavelength structures (the scale is hundreds of nanometers) such as a fine ripple periodic structure, a coarse ripple periodic structure and the like are respectively induced at different positions of the micron-sized structure. Meanwhile, the corrugated structures with different periods and depths can be obtained on the side wall of the micron-sized structure by changing the laser energy density, the defocusing amount, the scanning speed and the like; by changing the direction of the scanning speed, different angles can be formed with the polarization direction of the laser, thereby obtaining different ripple orientations. The micron-sized structure array obtained by combining the laser assisted water jet can obtain a multi-level layered structure. After silanization treatment, the surface reaches a Cassie-Baxter state, and the contact angle between the liquid drop and the surface of the monocrystalline silicon is increased, so that hydrophobicity or even superhydrophobicity is obtained.
In some embodiments, a pulsed fiber laser that emits nanosecond laser light with a center wavelength of 1064nm is employed in laser-assisted water jet processing.
In some embodiments, the process of laser assisted water jet machining includes the steps of:
adjusting the water jet impact angle, the water jet offset distance and the nozzle target distance;
Regulating the water jet pressure;
setting laser pulse width, pulse repetition frequency, laser power and scanning speed;
And writing a scanning track file according to the scanning direction and the scanning interval, running a machining program to finish machining in the horizontal direction, and then automatically rotating the workpiece to repeat the operation to finish machining in the vertical direction, so as to construct the micrometer-scale structure array.
In one or more embodiments, the water jet impingement angle is 40 ° to 50 °, the water jet offset distance is 0.4 to 0.6mm, and the nozzle target distance is 0.4 to 0.6mm.
In one or more embodiments, the water jet pressure is between 6 and 10MPa.
In one or more embodiments, the laser pulse width is 10-350 ns, the pulse repetition frequency is 20-1000 kHz, the laser power is 10-20W, and the scanning speed is 1-3 mm/s.
In some embodiments, the femtosecond laser has a center wavelength of 800nm, a pulse width of 35fs, and a repetition rate of 1kHz. The femtosecond laser is a gaussian beam.
In some embodiments, the process of femtosecond laser induced low frequency periodic surface structure includes the steps of:
Setting laser power and repetition frequency according to an ablation threshold value of a material;
adjusting the scanning direction, the scanning speed and the scanning interval according to the processing track to form a processing track file;
Adjusting the defocus amount;
And (5) running the machining track file to finish automatic machining.
In one or more embodiments, the laser power is 2.91 to 7.10 μW.
In one or more embodiments, the scan speed is 200-400 μm/s and the scan pitch is 38-78 μm.
In one or more embodiments, the defocus amount is +60 to +120 μm.
In some embodiments, the hydrophobic silane is perfluorodecyl triethoxysilane. The soaking time is 12-36 h.
In another embodiment of the invention, monocrystalline silicon with a hydrophobic functional surface is provided, which is obtained by the preparation method.
In some embodiments, the surface water contact angle is 130 ° to 153 °.
In a third embodiment of the invention, there is provided the use of monocrystalline silicon with a hydrophobic functional surface in the photovoltaic, microelectronics and/or biomedical fields.
In particular for the preparation of silicon-based solar cells or microelectromechanical systems.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail with reference to specific embodiments.
Example 1
As shown in fig. 1, the preparation method of the single crystal silicon micro-nano double-scale antireflection suede comprises the following steps:
1. The method for preparing the micron-sized matrix structure array by laser-assisted water jet processing adopts laser with the wavelength of 1064nm and comprises the following specific steps:
(1) The water jet impact angle is adjusted to be 42 degrees, the water jet offset distance is 0.5mm, and the nozzle target distance is 0.4mm.
(2) And adjusting the water jet pressure to 8MPa.
(3) Setting the laser pulse width to 10ns, the pulse repetition frequency to 1000kHz, the laser power to 15W and the scanning speed to 3mm/s.
(4) Selecting a scanning interval of 40 mu m, writing a scanning track file, then running a machining program to sequentially finish machining in the horizontal direction, then automatically rotating a workpiece by 90 degrees, and running the machining program to finish machining in the vertical direction, wherein the constructed micron-sized rectangular structure array is shown in fig. 2 (a), and the depth of a micro groove is 7.2 mu m, and the width of the micro groove is 22.1 mu m.
2. Inducing a surface periodic structure array by using femtosecond laser near an ablation threshold on the basis of a micron-level rectangular structure array, and adopting the femtosecond laser with the center wavelength of 800nm, the pulse width of 35fs and the repetition frequency of 1kHz, wherein the femtosecond laser is a Gaussian beam, and the specific steps are as follows:
(1) The laser power will be set to 2.91 mu W around the ablation threshold of the material.
(2) The scanning speed was set at 200 μm/s and the scanning pitch was set at 54. Mu.m, so that a processing track file was generated.
(3) The defocus amount was adjusted to +80. Mu.m.
(4) And the scanning is completed by running the processing track file, the obtained periodic structure morphology of the uniform surface of the micron-sized matrix structure is shown as a figure 3, and the low-frequency periodic surface structure with the direction perpendicular to the laser polarization E is uniformly distributed on the surface of the micron-sized structure. After 24 hours of immersion in the perfluorodecyl triethoxysilane solution, the contact angle is 134 ° as measured by a contact angle meter.
Example 2
As shown in fig. 1, the preparation method of the single crystal silicon micro-nano double-scale antireflection suede comprises the following steps:
1. The method for preparing the micron-sized matrix structure array by laser-assisted water jet processing adopts laser with the wavelength of 1064nm and comprises the following specific steps:
(1) The water jet impact angle is adjusted to 45 degrees, the water jet offset distance is 0.6mm, and the nozzle target distance is 0.6mm.
(2) And adjusting the water jet pressure to 6MPa.
(3) The pulse width of the laser is set to 100ns, the pulse repetition frequency is 144kHz, the laser power is 20W, and the scanning speed is 1mm/s.
(4) The scanning interval is 40 mu m, a processing program is operated to finish the processing in the vertical direction after the scanning track file is written, and the constructed micron-sized V-shaped groove structure array is shown in the figure 2 (b), wherein the depth of the micro groove is 20.6 mu m, and the width of the micro groove is 37.5 mu m.
2. Inducing a surface periodic structure array by using femtosecond laser near an ablation threshold on the basis of a micron-level rectangular structure array, and adopting the femtosecond laser with the center wavelength of 800nm, the pulse width of 35fs and the repetition frequency of 1kHz, wherein the femtosecond laser is a Gaussian beam, and the specific steps are as follows:
(1) The laser power will be set to 2.91 mu W around the ablation threshold of the material.
(2) The scanning speed was set at 300 μm/s and the scanning pitch was set at 38 μm, so that a processing track file was generated.
(3) The defocus amount was adjusted to +60. Mu.m.
(4) And the scanning is completed by running the processing track file, the obtained periodic structure morphology of the uniform surface of the micron-sized matrix structure is shown as a figure 4, and the low-frequency periodic surface structure with the direction perpendicular to the laser polarization E is uniformly distributed on the surface of the micron-sized structure. After soaking for 24 hours by using a perfluorodecyl triethoxysilane solution, the contact angle is 153 degrees and the super-hydrophobic performance is realized.
Example 3
As shown in fig. 1, the preparation method of the single crystal silicon micro-nano double-scale antireflection suede comprises the following steps:
1. The method for preparing the micron-sized matrix structure array by laser-assisted water jet processing adopts laser with the wavelength of 1064nm and comprises the following specific steps:
(1) The water jet impact angle is adjusted to 48 degrees, the water jet offset distance is 0.4mm, and the nozzle target distance is 0.5mm.
(2) And adjusting the water jet pressure to 10MPa.
(2) Setting the laser pulse width to 350ns, the pulse repetition frequency to 100kHz, the laser power to 10W and the scanning speed to 2mm/s.
(3) The scanning interval is 40 mu m, a processing program is operated to finish the processing in the vertical direction after the scanning track file is written, and the constructed micron-sized V-shaped groove structure array is shown in a figure 2 (c), wherein the depth of the micro groove is 10.6 mu m, and the width of the micro groove is 23.2 mu m.
2. Inducing a surface periodic structure array by using femtosecond laser near an ablation threshold on the basis of a micron-level rectangular structure array, and adopting the femtosecond laser with the center wavelength of 800nm, the pulse width of 35fs and the repetition frequency of 1kHz, wherein the femtosecond laser is a Gaussian beam, and the specific steps are as follows:
(1) The laser power will be set to 7.10 mu W around the ablation threshold of the material.
(2) The scanning speed was set at 400 μm/s and the scanning pitch was set at 78 μm to generate a processing track file.
(3) The defocus amount was adjusted to +120. Mu.m.
(4) And the scanning is completed by running the processing track file, the obtained periodic structure morphology of the uniform surface of the micron-sized matrix structure is shown in fig. 5, and the low-frequency periodic surface structure with the direction perpendicular to the laser polarization E is uniformly distributed on the surface of the micron-sized structure. After 24 hours of immersion in the perfluorodecyl triethoxysilane solution, the contact angle is 130 ° as measured by a contact angle meter.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of monocrystalline silicon with a hydrophobic functional surface is characterized in that laser-assisted water jet processing is carried out on the monocrystalline silicon surface, so that a micron-sized V-shaped groove structure array is formed on the monocrystalline silicon surface; forming a nano structure on the surface of the micron-sized V-shaped groove structure array by using the femtosecond laser to induce a low-frequency periodic surface structure, inducing a fine ripple periodic structure and a coarse ripple periodic structure, and changing the scanning speed direction to obtain different ripple orientations so as to form a micro-nano double-scale layered structure on the surface of the monocrystalline silicon; immersing monocrystalline silicon with a micro-nano double-scale layered structure on the surface into hydrophobic silane for silanization treatment, thus obtaining the silicon nitride; in the laser-assisted water jet processing, water jet is placed in the laser along the scanning speed direction;
in the laser-assisted water jet processing, a pulse fiber laser which emits laser with the center wavelength of 1064 nm nanoseconds is adopted;
The laser assisted water jet machining process comprises the following steps:
adjusting the water jet impact angle, the water jet offset distance and the nozzle target distance;
Regulating the water jet pressure;
setting laser pulse width, pulse repetition frequency, laser power and scanning speed;
writing a scanning track file according to the scanning direction and the scanning interval, running a machining program to finish machining in the horizontal direction, and then automatically rotating the workpiece to repeat the operation to finish machining in the vertical direction, so as to construct a micron-sized structure array;
The impact angle of the water jet is 40-50 degrees, the offset distance of the water jet is 0.4-0.6 mm, and the target distance of the nozzle is 0.4-0.6 mm;
The water jet pressure is 6-10 MPa;
the laser pulse width is 10-350 ns, the pulse repetition frequency is 20-1000 kHz, the laser power is 10-20W, and the scanning speed is 1-3 mm/s;
The process of inducing the low-frequency periodic surface structure by the femtosecond laser comprises the following steps:
Setting laser power and repetition frequency according to an ablation threshold value of a material;
adjusting the scanning direction, the scanning speed and the scanning interval according to the processing track to form a processing track file;
Adjusting the defocus amount;
The automatic processing is completed by running a processing track file;
The laser power is 2.91-7.10 mu W;
The scanning speed is 200-400 mu m/s, and the scanning interval is 38-78 mu m;
The defocusing amount is +60 to +120 mu m.
2. The method for producing a silicon single crystal having a hydrophobic functional surface according to claim 1, wherein the femtosecond laser has a center wavelength of 800nm, a pulse width of 35fs, and a repetition frequency of 1kHz.
3. The method for producing a single crystal silicon having a hydrophobic functional surface according to claim 1, wherein the hydrophobic silane is perfluorodecyl triethoxysilane.
4. The method for producing a silicon single crystal having a hydrophobic functional surface according to claim 3, wherein the soaking time is 12 to 36 hours.
5. A single crystal silicon having a hydrophobic functional surface, characterized by being obtained by the method for producing a single crystal silicon having a hydrophobic functional surface as claimed in any one of claims 1 to 4.
6. The silicon single crystal having a hydrophobic functional surface according to claim 5, wherein the surface water contact angle is 130 ° to 153 °.
7. Use of monocrystalline silicon with a hydrophobic functional surface according to claim 5 or 6 in the photovoltaic or microelectronics or biomedical field.
8. Use according to claim 7, in the preparation of silicon-based solar cells or microelectromechanical systems.
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| CN108526627A (en) * | 2018-06-27 | 2018-09-14 | 江苏大学 | A kind of semi-conducting material laser electrochemical copolymerization micro-processing method and device |
| CN111673285A (en) * | 2020-06-30 | 2020-09-18 | 吉林大学 | Method for forming micro-nano multilayer structure on amorphous carbon surface through nanosecond laser irradiation induction |
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| EP2253413A1 (en) * | 2009-05-15 | 2010-11-24 | National University of Ireland Galway | Method for laser ablation |
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| CN108526627A (en) * | 2018-06-27 | 2018-09-14 | 江苏大学 | A kind of semi-conducting material laser electrochemical copolymerization micro-processing method and device |
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