CN111229719B - Method for preparing multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance - Google Patents
Method for preparing multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance Download PDFInfo
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- CN111229719B CN111229719B CN202010103694.7A CN202010103694A CN111229719B CN 111229719 B CN111229719 B CN 111229719B CN 202010103694 A CN202010103694 A CN 202010103694A CN 111229719 B CN111229719 B CN 111229719B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
- B08B7/0042—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like by laser
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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
- B23K26/36—Removing material
- B23K26/362—Laser etching
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Abstract
A method for preparing a multi-scale micro-nano composite structure through laser cleaning and laser ablation assistance comprises the steps of building a light path, enabling output light of a femtosecond laser to enter a scanning galvanometer after passing through a reflecting mirror, irradiating the output light on an objective table after being focused by a round lens of the scanning galvanometer, and connecting the femtosecond laser, the scanning galvanometer and a computer; setting parameters for laser ablation of silicon materials, and fixing a monocrystalline silicon wafer sample on a movable objective table; the computer controls the scanning galvanometer to realize the cross grid movement of laser spots, and the surface of a grid-shaped micron structure covered with a layer of flocculent oxide deposit is obtained after the surface of the monocrystalline silicon wafer sample is ablated by laser; replacing a circular lens of the scanning galvanometer with a cylindrical lens to obtain an elliptical light spot; setting parameters for cleaning silicon oxide deposition by laser, controlling a scanning galvanometer by a computer to realize grid-shaped movement of laser spots, and cleaning the surface of the grid-shaped micro-structure by the laser to prepare a multi-scale micro-nano composite structure; the method is simple to operate, green, environment-friendly, economical and efficient.
Description
Technical Field
The invention belongs to the technical field of micro-nano structure preparation, and particularly relates to a method for preparing a multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance.
Background
The silicon-based wave-absorbing material has a huge application market in the fields of aerospace, national defense and military, new energy and the like. The solar cell can be made in a visible light wave band; a photoelectric detector can be made in an infrared band; the terahertz wave band can be used as an absorber and a radiation source. Therefore, an anti-reflection structure is manufactured on the surface of the silicon material by utilizing an ultrafast laser processing technology, the silicon material can efficiently absorb electromagnetic waves, and the method has important significance for the production life of people and the national defense and military.
The existing research shows that the multi-scale micro-nano composite structure not only can exert the advantages of a micro-structure and a nano-structure to improve the wave-absorbing efficiency, but also can effectively widen the absorbed frequency spectrum range due to the multi-level characteristic, so that the broadband wave-absorbing performance of the silicon material surface can be improved by preparing the multi-scale micro-nano structure on the silicon material surface by using femtosecond laser. However, the silicon material is processed by laser in the air, ablation deposition particles generated by laser ablation of the silicon material can be oxidized into silicon dioxide, so that the surface of the silicon material is covered with a layer of flocculent oxide, and the wave-absorbing property is greatly reduced. The existing solution is to carry out laser processing on silicon in an inert gas environment, the equipment is complex, the processing cost is greatly improved, and simultaneously, the generated waste gas causes environmental pollution. Therefore, how to prepare the multi-scale micro-nano composite structure on the surface of the silicon material in a green and efficient manner to improve the wave absorbing performance of the surface of the material becomes a difficult problem to be solved urgently.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the method for preparing the multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance, which can realize the preparation of the multi-scale micro-nano composite structure comprising the micron structure, the submicron structure and the nano structure in the air, improve the wave-absorbing performance of the surface of the material, and has the advantages of simple processing method operation, environmental protection, economy and high efficiency.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance comprises the following steps:
1) respectively carrying out ultrasonic cleaning on the surface of a monocrystalline silicon wafer sample by using acetone and absolute ethyl alcohol, and drying by using cold air to obtain a clean monocrystalline silicon wafer sample surface;
2) the method comprises the following steps of building a light path, wherein the light path comprises a femtosecond laser, the output light of the femtosecond laser enters a scanning galvanometer after passing through a reflector, the light is focused by a round lens of the scanning galvanometer and then irradiates on an objective table, the femtosecond laser, the scanning galvanometer and a computer are connected, the focal length of the round lens is 170mm, and the diameter of a focusing round light spot is 30 micrometers;
3) adjusting the output laser wavelength of the femtosecond laser to 1030nm, the repetition frequency to 50kHz, the pulse width to 240fs and the laser power to 800mW by using a computer;
4) fixing a monocrystalline silicon wafer sample on a processing station of a movable objective table;
5) controlling a scanning galvanometer by a computer to realize the cross grid movement of laser spots, wherein the movement distance is 50 mu m, the movement speed is 5mm/s, and the surface of a latticed microstructure covered with a layer of flocculent oxide deposit is obtained after the surface of a monocrystalline silicon wafer sample is ablated by laser;
6) replacing a circular lens of a scanning galvanometer with a cylindrical lens, and using the cylindrical lens with the focal length of 75mm for focusing a circular light spot laser beam output by a femtosecond laser to obtain an elliptical light spot, wherein the major axis size radius of the light spot is 2mm, and the minor axis size radius is 10 mu m;
7) adjusting the output laser wavelength of the femtosecond laser to 1030nm, the repetition frequency to 10kHz, the pulse width to 240fs and the laser power to 60mW by using a computer;
8) and controlling a scanning galvanometer by using a computer to realize grid-shaped movement of laser spots, wherein the movement distance is 10 mu m, the movement speed is 10mm/s, and the surface of a latticed microstructure covered with a layer of flocculent oxide deposit is cleaned by laser, so that the multi-scale micro-nano composite structure of the microstructure, the submicron structure and the nano structure is prepared.
The invention has the beneficial effects that: the invention provides a method for preparing a multi-scale micro-nano structure in air by laser cleaning assisted laser ablation, which utilizes the characteristic that the laser ablation threshold of silicon oxide deposition is smaller than the ablation threshold of a silicon material, applies a laser cleaning mechanism, selects laser energy equal to the ablation threshold of the silicon material, cleans and removes oxide deposition covered on the surface of a silicon micro-structure prepared by laser ablation, and simultaneously can induce submicron and nano structures on the surface of the micro-structure by laser cleaning, thereby preparing the multi-scale micro-nano composite structure and improving the wave-absorbing performance of the surface of the material. The method solves the problems that the silicon surface is prevented from being oxidized by the traditional laser processing method and needs to be processed in a protective gas environment, and is green, economic, convenient and feasible.
Drawings
FIG. 1 is a schematic view of femtosecond laser processing according to the present invention.
Fig. 2 is a result graph of a grid micro-nanostructure covered with oxide deposition prepared by laser ablation in embodiment 1 of the present invention.
Fig. 3 is a schematic diagram of a cylindrical lens according to the present invention.
Fig. 4 is a result graph of the multi-scale micro-nano composite structure prepared after laser cleaning in embodiment 1 of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
A method for preparing a multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance comprises the following steps:
1) carrying out ultrasonic cleaning on the surface of a monocrystalline silicon wafer sample 7 by using acetone and absolute ethyl alcohol respectively, and drying by using cold air to obtain a clean monocrystalline silicon wafer sample surface;
2) building a light path, referring to fig. 1, wherein the light path comprises a femtosecond laser 1, output light of the femtosecond laser 1 enters a scanning galvanometer 5 after passing through a first reflecting mirror 2, a second reflecting mirror 3 and a third reflecting mirror 4, the light is focused by a round lens 6 of the scanning galvanometer 5 and then irradiates an objective table 8, the femtosecond laser 1 and the scanning galvanometer 5 are connected with a computer, the focal length of the round lens 6 is 170mm, and the diameter of a focusing round light spot is 30 μm;
3) adjusting the output laser wavelength of the femtosecond laser 1 to 1030nm, the repetition frequency to 50kHz, the pulse width to 240fs and the laser power to 800mW by using a computer;
4) fixing a monocrystalline silicon wafer sample 7 on a processing station of a movable objective table 8;
5) controlling a scanning galvanometer 5 by a computer to realize the cross grid movement of laser spots, wherein the movement distance is 50 mu m, the movement speed is 5mm/s, and after the surface of a monocrystalline silicon wafer sample 7 is ablated by laser, the surface of a grid-shaped microstructure covered with a layer of flocculent oxide deposition is obtained, as shown in figure 2, a regular square grid micron-sized structure is prepared on the surface, microgrooves with large depth ratio exist around the microstructure, and meanwhile, a layer of flocculent nanoscale oxide deposition is covered on the surface of the microstructure;
6) replacing the circular lens 6 of the scanning galvanometer 5 with a cylindrical lens 9, as shown in fig. 3, using the cylindrical lens 9 with a focal length of 75mm for focusing the circular spot laser beam output by the femtosecond laser 1 to obtain an elliptical spot, wherein the major axis dimension radius of the spot is 4mm, and the minor axis dimension radius is 10 μm;
7) adjusting the output laser wavelength of the femtosecond laser 1 to 1030nm, the repetition frequency to 10kHz, the pulse width to 240fs and the laser power to 80mW by using a computer;
8) the scanning galvanometer 5 is controlled by a computer to realize grating movement of laser spots, the movement distance is 10 microns, the movement speed is 10mm/s, the laser cleans the surface of a latticed microstructure covered with a layer of flocculent oxide deposit, namely, a multi-scale micro-nano composite structure of a microstructure, a submicron structure and a nano structure is prepared, as shown in figure 4, the flocculent oxide deposit on the surface of the square lattice microstructure is removed, the surface of a material is prepared into a square lattice structure of a micron scale, a groove structure of a micron scale, a hole pattern and a protruding structure of a submicron scale, gaps and particles of a nano scale, and the multi-scale micro-nano composite structure is formed on the surface of the material.
Claims (1)
1. A method for preparing a multi-scale micro-nano composite structure by laser cleaning and laser ablation assistance is characterized by comprising the following steps:
1) respectively carrying out ultrasonic cleaning on the surface of a monocrystalline silicon wafer sample by using acetone and absolute ethyl alcohol, and drying by using cold air to obtain a clean monocrystalline silicon wafer sample surface;
2) the method comprises the following steps of building a light path, wherein the light path comprises a femtosecond laser, the output light of the femtosecond laser enters a scanning galvanometer after passing through a reflector, the light is focused by a round lens of the scanning galvanometer and then irradiates on an objective table, the femtosecond laser, the scanning galvanometer and a computer are connected, the focal length of the round lens is 170mm, and the diameter of a focusing round light spot is 30 micrometers;
3) adjusting the output laser wavelength of the femtosecond laser to 1030nm, the repetition frequency to 50kHz, the pulse width to 240fs and the laser power to 800mW by using a computer;
4) fixing a monocrystalline silicon wafer sample on a processing station of a movable objective table;
5) controlling a scanning galvanometer by a computer to realize the cross grid movement of laser spots, wherein the movement distance is 50 mu m, the movement speed is 5mm/s, and the surface of a latticed microstructure covered with a layer of flocculent oxide deposit is obtained after the surface of a monocrystalline silicon wafer sample is ablated by laser;
6) replacing a circular lens of a scanning galvanometer with a cylindrical lens, and using the cylindrical lens with the focal length of 75mm for focusing a circular light spot laser beam output by a femtosecond laser to obtain an elliptical light spot, wherein the major axis size radius of the light spot is 2mm, and the minor axis size radius is 10 mu m;
7) adjusting the output laser wavelength of the femtosecond laser to 1030nm, the repetition frequency to 10kHz, the pulse width to 240fs and the laser power to 60mW by using a computer;
8) and controlling a scanning galvanometer by using a computer to realize grid-shaped movement of laser spots, wherein the movement distance is 10 mu m, the movement speed is 10mm/s, and the surface of a latticed microstructure covered with a layer of flocculent oxide deposit is cleaned by laser, so that the multi-scale micro-nano composite structure of the microstructure, the submicron structure and the nano structure is prepared.
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| CN111992543B (en) * | 2020-08-21 | 2021-10-22 | 厦门理工学院 | Laser plasma light wire cleaning method |
| CN112355484B (en) * | 2020-09-28 | 2022-10-18 | 天津津航技术物理研究所 | Surface periodic conical microstructure processing method based on Gaussian beam focusing direct writing |
| CN115000203B (en) * | 2022-06-20 | 2023-11-21 | 山东大学 | Single crystal silicon micro-nano double-scale antireflection suede and preparation method thereof |
| CN115198243A (en) * | 2022-08-12 | 2022-10-18 | 南京理工大学 | Femtosecond laser pure additive device suitable for active easily-oxidized material |
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| CN100462181C (en) * | 2006-10-30 | 2009-02-18 | 西安交通大学 | Femto-second laser ture three-D micro-nano-processing center |
| CN102858512B (en) * | 2010-02-11 | 2016-12-07 | 谭永杰 | A kind of system and method for manufacturing microstructure |
| CN102529211B (en) * | 2011-12-22 | 2014-09-24 | 电子科技大学 | Film system structure for enhancing Terahertz radiation absorption rate and preparation method thereof |
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