CN107627025B - Preparation method of wide-bandgap crystal material surface micro-nano structure - Google Patents
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Abstract
The invention discloses a preparation method of a wide band gap crystal material surface micro-nano structure. Cleaning the selected wide band gap crystal material, and placing the cleaned wide band gap crystal material into a processing cavity, wherein the processing cavity can be in vacuum (the vacuum degree is 10)‑2‑10‑5Pa) or introducing gas with certain pressure (less than 1bar), wherein the gas can be etching gas such as sulfur hexafluoride, chlorine and the like, and can also be non-etching gas such as nitrogen, helium, argon and even air and the like. Then heating the sample (the temperature is 20-1500 ℃), and using ultrashort pulse laser (the wavelength can be from ultraviolet to near infrared, the pulse width can be 5fs-5000fs, and the flux range of the ultrashort pulse laser is 1kJ/m2‑100kJ/m2) And irradiating the surface of the sample to prepare a micro-nano structure. The invention solves the problem of coulomb explosion caused by irradiation of the wide-bandgap crystal material by ultrashort pulse laser at normal temperature, realizes the preparation of the surface micro-nano structure of the wide-bandgap crystal material, and can control the size of the micro-nano structure by controlling the energy of incident laser and irradiation time.
Description
Technical Field
The invention relates to the field of material processing, in particular to a method for processing a wide band gap crystal material by laser and realizing the processing of a micro-nano structure on the surface of the material. The method can be applied to the fields of ultrashort pulse laser processing, nanometer material processing, super-diffraction optical component manufacturing and photoelectric device manufacturing.
Background
The ultrashort pulse laser has the unique advantages of high peak power, small heat effect, high processing precision and the like, and is widely applied to the field of material processing. By using ultrashort pulse laser, a plurality of micron-scale and nanometer-scale structures, such as surface periodic stripes, cone-shaped structures, nanoparticles and the like, are prepared on the surface of the material. Modern researches show that the ultrashort pulse laser induces the micro-nano structure on the surface of the material to change the optical properties (reflection, absorption, photoluminescence and the like), the electrical properties (conductivity, electroluminescence and the like), the hydrophilicity or the hydrophobicity and the like of the material.
At present, the known methods for processing materials by ultrashort pulse laser are all performed at room temperature. For metals and some semiconductor materials with narrow band gaps, processing the materials by using ultrashort pulse laser in a room temperature environment is enough to achieve the expected effect, but for semiconductor materials and dielectric materials with wide band gaps, the ultrashort pulse laser is used for inducing the surface of the materials to form a periodic micro-nano structure in the room temperature environment, so that great difficulty exists. This is because, when the ultrashort pulse laser is irradiated to the surface of the material, the temperature of electrons may sharply rise within several femtoseconds; when the kinetic energy of the electrons exceeds the binding energy of the electrons, the electrons escape. After the electrons escape, a large number of holes are left, and thus the surface of the material is positively charged. Since the entire lattice is in a tightly bound state at room temperature and the conductivity of the wide band gap material is low, it is impossible to compensate the surface by diffusion of electrons and holes inside the material, which results in gradual localization of the surface. In a localized small volume, due to the strong coulomb repulsion between positive charges, a large amount of ion beams are sputtered to neutralize the positive charges on the surface of the material. At this time, a pit-shaped structure is formed on the surface of the material due to the fact that a large amount of material is sputtered out, and therefore the assumption that the periodic micro-nano structure is prepared on the surface of the wide-band gap crystal material by the ultrashort pulse laser cannot be realized.
Many researchers have encountered such difficulties. Industrial university of kodbury blandburg, germany, group of subjects j.reif, using ultra-short pulsed laser on Al2O3、NaCl、BaF2Processing the surface of the crystal with the equal-width band gapThe coulomb explosion phenomenon also occurs on the surface of the material. This phenomenon, which is caused by the properties of the material itself, can cause great difficulties in material processing and application. Therefore, a method for processing a micro-nano structure on the surface of a wide band gap crystal material is urgently needed to be found.
Disclosure of Invention
In order to solve the above problems, the present inventors have made long-term experiments and studies to provide a new processing method, which can overcome the defects of the existing ultrashort pulse laser processing technology in processing a wide bandgap crystal material, solve the difficulties caused by the material characteristics, and finally realize the concept of using ultrashort pulse laser to prepare a micro-nano structure on the surface of the wide bandgap crystal material.
According to the technical scheme of the invention, the preparation method of the periodic micro-nano structure on the surface of the wide band gap crystal material is provided, and comprises the following steps:
step 1: selecting a wide-band-gap crystal material, and cleaning the surface of the material in an ultrasonic or wiping mode;
step 2: fixing a cleaned sample on a sample support, wherein the sample support is fixed on a three-dimensional moving platform, namely, the sample can move randomly in a two-dimensional plane vertical to the incident laser direction by controlling the moving platform;
and step 3: heating the sample by using a heating table, so that the temperature of the sample is adjustable within the range of 20-1500 ℃;
and 4, step 4: setting the area of a sample processing area and the scanning speed in a control window of a three-dimensional mobile platform;
and 5: placing a sample in a processing cavity, adjusting the power of incident laser to an appropriate value, and irradiating the surface of the wide-bandgap crystal material with ultrashort pulse laser to prepare a periodic micro-nano structure;
step 6: after the processing is finished, when the temperature of the sample is reduced to room temperature, introducing nitrogen or air into the processing cavity, vacuumizing when the air pressure in the processing cavity reaches a standard atmospheric pressure, wherein the vacuum degree is 100-10-5Introducing nitrogen or air again between Pa, extracting, inflating and extractingMultiple cycles are carried out, gas is filled into the processing cavity at the moment, and when the air pressure in the cavity reaches a standard atmospheric pressure, the cavity cover is opened, and the sample is taken out
Thus, the preparation of the surface micro-nano structure of the wide band gap crystal material under the high temperature condition is completed.
The wide band gap crystal material in the step 1 is a semiconductor material or a dielectric material, the crystal orientation, the size and the thickness of the wide band gap crystal material are not limited, the wide band gap crystal material can be selected according to actual conditions, the crystal material is required to be smooth, and the surface smoothness of the wide band gap crystal material, namely the difference value between the highest point and the lowest point of the surface of the material, is less than or equal to 10 micrometers;
preferably, the rear end of the sample heating table described in step 3 is fixed to the three-dimensional moving platform, the front end of the sample heating table is used for fixing the sample holder, and the movement of the sample is realized through intelligent control of the three-dimensional moving platform;
preferably, when the ultrashort pulse laser irradiates the surface of the wide-bandgap crystal material in step 4, the speed of the mobile platform needs to ensure that when the ultrashort pulse laser irradiates the wide-bandgap crystal material sample, the unit area of the sample surface can receive irradiation of 1-5000 pulses, where the unit area refers to an area of a single pulse projected onto the sample surface when the ultrashort pulse laser irradiates the sample surface;
preferably, when the ultrashort pulse laser irradiates the surface of the wide band gap crystal material in the step 5,
(1) in vacuum or gas atmosphere with a vacuum degree of 100-10-5Pa, or introducing gas with certain pressure, wherein the gas comprises etching gas sulfur hexafluoride, chlorine or non-etching gas nitrogen, helium, argon and air;
(2) irradiating the surface of the sample with ultrashort pulse laser with wavelength ranging from ultraviolet to near infrared and pulse width of 5-5000 fs and flux of 1kJ/m2-100kJ/m2In the processing process, a sample on the sample support is driven by a three-dimensional moving platform to perform two-dimensional scanning on a plane vertical to incident laser, so that a micro-nano structure is prepared on the surface of the wide-bandgap crystal material;
(3) after the ultrashort pulse laser processing, the surface of the crystal material can be etched by laser to form a surface micro-nano structure, and the size of a single micro-structure is 50nm-10 mu m.
Has the advantages that:
1. the preparation method of the periodic micro-nano structure on the surface of the wide band gap crystal material provided by the invention has the advantages of simple process, easiness in control and the like.
2. The invention utilizes the heating table to heat the sample, and also utilizes the heating table to control the cooling rate of the sample, thereby eliminating the defects caused in the processing process and effectively maintaining the lattice structure of the wide-band-gap crystal material.
3. According to the processing of the wide band gap crystal material in the gas, provided by the invention, gas elements can be doped into the material, so that high-concentration doping of the wide band gap crystal material is realized.
4. After the temperature is reduced to room temperature, gas is introduced, so that the material can be effectively prevented from being oxidized by the gas at high temperature.
5. After the processing is finished, the nano particles generated in the processing process can be discharged out of the vacuum cavity along with the gas through multiple times of inflation and air exhaust, and the harm to the body caused by the suction of an operator is prevented.
Drawings
FIG. 1 is a flow chart of ultra-short pulse laser processing of wide bandgap crystalline materials.
FIG. 2 is a schematic diagram of ultrashort pulse laser processing of wide bandgap crystalline materials.
FIG. 3 is a schematic diagram of the structure of the sample heating stage.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to illustrate the technical means and efficacy of the invention in more detail, the method for preparing the surface micro-nano structure of the wide band gap crystalline material provided by the invention is described in detail below with reference to examples.
The preparation method of the invention is further explained below with reference to the accompanying drawings.
FIG. 1 is a schematic flow chart of preparation of a wide band gap material surface micro-nano structure.
FIG. 2 is a schematic diagram of ultrashort pulse laser processing of wide bandgap crystalline materials. In the attached figure 2, 2-1 is ultrashort pulse laser, 2-2 is a 50cm convex lens, 2-3 is a processing cavity, 2-4 is a sample heating table, and 2-5 is a three-dimensional moving platform. The crystal material is arranged in a vacuum cavity and fixed on a sample support, and ultrashort pulse laser irradiates the surface of the material through a focusing lens. The sample holder is connected with a three-dimensional moving platform controlled by a computer, and can move two-dimensionally on a plane vertical to the incident laser in the processing process.
FIG. 3 is a block diagram of a sample heating stage. 3-1 is a sample support, 3-2 is a sample heating table, the rear end is fixed on a three-dimensional moving platform, the front end can be fixed with the sample support, and 3-3 is a thermocouple wire for detecting the temperature of the sample in real time.
Examples of the embodiments
The preparation method of the surface micro-nano structure of the wide band gap crystal material comprises the following steps:
1. selecting a z-tangential iron-doped lithium niobate crystal as a target material, wherein the area of the target material is 1 × 1cm2The thickness is 1 mm;
2. the lithium niobate crystal slice is ultrasonically cleaned for 15 minutes in mixed solution of ethanol and acetone with the volume ratio of 1: 1, and then is washed by a large amount of deionized water, so that the surface is clean.
3. Fixing the cleaned lithium niobate thin sheet on 1.2 × 1.2.2 cm by using a small screw2The sample holder is fixed at the front end of the sample heating platform, and the rear end of the sample holder is connected with the three-dimensional moving platform, so that the sample can be controlled by the three-dimensional moving platform.
4. Vacuum pumping is carried out, and the vacuum degree is 10-2Pa。
5. Setting a temperature rising program section, namely a first section: heating to 1000 deg.C for 120 min; and a second stage: maintaining the temperature at 1000 deg.C for 30min for processing the material; a third stage: the temperature is reduced to 200 ℃.
6. The wavelength of the ultrashort pulse laser is 800nm, the pulse width is 120fs, and the laser power is adjusted to ensure that the flux of the ultrashort pulse laser irradiated to the surface of the sample is 6kJ/m2。
7. Setting the moving speed at 1mm/s and the line spacing at 100 μm in the control window of the three-dimensional moving translation stage, and performing surface scanning with a scanning area of 0.8 × 0.8.8 cm2. After the processing is finished, when the temperature of the sample is reduced to room temperature, introducing nitrogen or air into the processing cavity, and vacuumizing to 10 ℃ when the air pressure in the processing cavity reaches a standard atmospheric pressure-2And Pa, introducing nitrogen or air again, exhausting, inflating and exhausting, circulating for 3 times, then inflating gas into the processing cavity, and opening the cavity cover and taking out the sample when the air pressure in the cavity reaches a standard atmospheric pressure.
Thus finishing the preparation of the micro-nano structure on the surface of the iron-doped lithium niobate crystal material under the high-temperature condition.
It should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments. It will be apparent to those skilled in the art that other variations and modifications may be made in the invention without departing from the spirit or scope of the invention as defined in the following claims. Obvious variations or modifications of this invention are within the scope of the invention as claimed.
Claims (1)
1. A preparation method of a wide band gap crystal material surface micro-nano structure is characterized by comprising the following steps:
step 1: selecting a wide-band-gap crystal material, and cleaning the surface of the material in an ultrasonic or wiping mode;
step 2: fixing a cleaned sample on a sample support, wherein the sample support is fixed on a three-dimensional moving platform, namely, the sample can move randomly in a two-dimensional plane vertical to the incident laser direction by controlling the moving platform;
and step 3: heating the sample by using a heating table, so that the temperature of the sample is adjustable within the range of 20-1500 ℃;
and 4, step 4: setting the area of a sample processing area and the scanning speed in a control window of a three-dimensional mobile platform;
and 5: placing a sample in a processing cavity, adjusting the power of incident laser to an appropriate value, and irradiating the surface of the wide-bandgap crystal material with ultrashort pulse laser to prepare a periodic micro-nano structure;
step 6: after the processing is finished, when the temperature of the sample is reduced to room temperature, introducing nitrogen or air into the processing cavity, vacuumizing when the air pressure in the processing cavity reaches a standard atmospheric pressure, wherein the vacuum degree is 100-10-5Introducing nitrogen or air again between Pa, exhausting, inflating and exhausting for multiple cycles, then inflating the processing cavity with gas, and opening the cavity cover and taking out the sample when the pressure in the cavity reaches a standard atmospheric pressure;
in step 1, the wide band gap crystal material is a semiconductor material or a dielectric material, the crystal orientation, size and thickness of the wide band gap crystal material are not limited, the wide band gap crystal material can be selected according to actual conditions, the crystal material is required to be smooth, and the surface smoothness of the wide band gap crystal material, namely the difference value between the highest point and the lowest point of the surface of the material, is less than or equal to 10 microns
In the step 3, the rear end of the sample heating table is fixed on the three-dimensional moving platform, the front end of the sample heating table is used for fixing the sample support, and the movement of the sample is realized through intelligent control on the three-dimensional moving platform; the speed of the mobile platform needs to ensure that 1-5000 pulse irradiations can be received on the unit area of the sample surface when the ultrashort pulse laser irradiates the wide-bandgap crystal material sample, wherein the unit area refers to the area of a single pulse projected on the sample surface when the ultrashort pulse laser irradiates the sample surface; the processing is carried out in vacuum or gas with a vacuum degree of 100-10-5Pa, or introducing gas with certain pressure, wherein the gas comprises etching gas sulfur hexafluoride, chlorine or non-etching gas nitrogen, helium, argon and air;
the mode and parameters of the ultrashort pulse laser irradiating the surface of the wide band gap crystal material in the step 5 are as follows: irradiating the surface of the sample with ultrashort pulse laser with wavelength ranging from ultraviolet to near infrared and pulse width of 5-5000 fs and flux of 1kJ/m2-100kJ/m2Has been processedIn the process, a sample on the sample support is driven by the three-dimensional moving platform to perform two-dimensional scanning on a plane vertical to incident laser; after the ultrashort pulse laser processing, the surface of the crystal material can be etched by laser to form a periodic surface microstructure, and the size of a single microstructure is 50nm-10 mu m.
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