CN111673285A - Method for forming micro-nano multilayer structure on amorphous carbon surface through nanosecond laser irradiation induction - Google Patents

Method for forming micro-nano multilayer structure on amorphous carbon surface through nanosecond laser irradiation induction Download PDF

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CN111673285A
CN111673285A CN202010606983.9A CN202010606983A CN111673285A CN 111673285 A CN111673285 A CN 111673285A CN 202010606983 A CN202010606983 A CN 202010606983A CN 111673285 A CN111673285 A CN 111673285A
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laser
amorphous carbon
micro
multilayer structure
nano multilayer
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CN111673285B (en
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黄虎
王超
钱永峰
崔明明
洪婧
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Jilin University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/352Working by laser beam, e.g. welding, cutting or boring for surface treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/60Preliminary treatment

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Abstract

The invention relates to a method for forming a micro-nano multilayer structure on an amorphous carbon surface through nanosecond laser irradiation induction, and belongs to the technical field of laser surface modification. The method comprises the following steps: ultrasonically cleaning the polished amorphous carbon sample by using absolute ethyl alcohol; performing light path conversion and focusing on laser generated by a nanosecond fiber laser by a galvanometer system, and then vertically irradiating the laser on the surface of the amorphous carbon sample; and controlling the irradiation time and energy density of laser pulses, and preparing the micro-nano multilayer structure on the surface of the amorphous carbon by utilizing the material removal effect of laser and the interference effect of light. The micro-nano multilayer structure comprises a micron-scale dimple-like structure and a nano-scale concentric ring-shaped structure. The method provided by the invention is simple and efficient, the formed surface microstructure is regular and well-arranged, a feasible method is provided for efficiently preparing the amorphous carbon surface micro-nano multilayer structure in a large area, and the method has wide application prospects in the fields of mold forming, surface wettability, optical characteristics, catalytic characteristic adjustment and the like.

Description

Method for forming micro-nano multilayer structure on amorphous carbon surface through nanosecond laser irradiation induction
Technical Field
The invention relates to the technical field of laser surface modification, in particular to a method for forming a micro-nano multilayer structure on an amorphous carbon surface through nanosecond laser irradiation induction. The invention can be applied to the fields of mold forming, surface wettability, optical property, catalytic property adjustment and the like to realize the processing of micro/nano multilayer structures.
Background
Amorphous carbon is an amorphous structure composed of SP2 hybrid atoms, has isotropic physicochemical properties, and has the characteristics common to carbon materials, such as good thermal stability, wear resistance, chemical inertness, and the like. In addition, amorphous carbon has excellent mechanical properties such as high hardness, Young's modulus, and the like. Due to these characteristics, amorphous carbon is widely used as a material for a hot press molding die for precision glass instruments and metals. At present, the processing methods for amorphous carbon include plasma reactive etching, focused ion beam milling, polymer molding carbonization, laser micro-milling and the like. Although the micro-nano-grade amorphous carbon mold has been successfully prepared by the processing methods, the preparation process of the methods is relatively complicated, the formed structure is simple, and the micro-nano composite structure is difficult to process. For example, in the method of preparing amorphous carbon molds proposed by Karin Prater in 2016 (Optical Materials Express, volume 6, 3407) 3416 (Micro-structural of glass carbon for precision glass molding of composite differential Optical elements), although some simple structures can be prepared, multilayer composite structures cannot be prepared. A large number of existing research results show that compared with a single surface structure, the micro-nano multilayer structure can more easily endow the surface of the material with special properties, such as improvement of hydrophobicity of the surface of the material, enhancement of optical absorption performance of the surface, improvement of surface catalytic performance and the like. For example, Venkata Krishan, International Journal of Heat and Mass Transfer, vol.140, 886-896 (Wettingtransition in laser-interfacial surface structures and sites immobilization magnet Transfer characteristics) in 2019, mentions the property of multilayer surface structures that can be used to enhance the superhydrophobic properties of material surfaces. However, it is still a difficult and critical issue to process micro-nano multilayer structures on the surfaces of different materials, and particularly, a new surface micro-nano multilayer structure processing method is urgently needed to be developed for a typical difficult-to-process material, amorphous carbon.
Laser processing is a processing mode with wide applicability, environmental protection and flexibility, and in recent years, femtosecond or picosecond lasers are widely applied to the creation of micro-nano composite structures on the surfaces of various materials. For example, Chenbin Ma in 2019, Journal of biological Engineering, volume 16, 806-813 (the Fabrication of systematic and high-performance structures on a 304 stationary step surface via a picosecond laser) prepared a micro-nano multilayer structure on the surface of 304stainless steel using a picosecond laser, which improves the surface hydrophobicity and adhesion properties. However, femtosecond or picosecond laser processing is more costly and less efficient. Compared with femtosecond or picosecond laser processing, nanosecond laser processing has the remarkable advantages of low cost, high efficiency and the like, and is more suitable for large-scale industrial application. Therefore, a new method for developing a preparation method of the amorphous carbon surface micro-nano multilayer structure is urgently needed based on nanosecond laser processing, and the method also has important practical application value.
Disclosure of Invention
The invention aims to provide a method for forming a micro-nano multilayer structure on the surface of amorphous carbon by nanosecond laser irradiation induction, which solves the problems in the prior art. The invention provides a feasible method for preparing a micro-nano multilayer structure on the surface of amorphous carbon, can prepare different structures such as single-point and multi-point arrays by controlling laser parameters, and has wide application prospects in the fields of mold forming, surface wettability, optical characteristics, catalytic characteristic regulation and the like.
The above object of the present invention is achieved by the following technical solutions:
a method for forming a micro-nano multilayer structure on an amorphous carbon surface through nanosecond laser irradiation induction is characterized in that point irradiation is carried out on the amorphous carbon surface in the air by controlling irradiation time and energy density of nanosecond laser pulses, and the micro-nano multilayer structure is prepared on the amorphous carbon surface by utilizing the material removal effect of laser and the interference effect of light, and comprises the following steps:
step one, carrying out ultrasonic cleaning and drying on the polished amorphous carbon sample by using absolute ethyl alcohol to obtain a pretreated amorphous carbon sample;
step two, performing light path conversion and focusing on laser generated by the nanosecond fiber laser through a galvanometer system, and then vertically irradiating the laser on the surface of the amorphous carbon sample obtained in the step one; by controlling the irradiation time and energy density of nanosecond laser pulse, the micro-nano multilayer structure is prepared on the surface of amorphous carbon by utilizing the material removal effect of laser and the interference effect of light.
And the cleaning temperature of the ultrasonic cleaning in the step one is 50-60 ℃, the cleaning time is 4-6min, and the ultrasonic cleaning is naturally dried in the air.
The laser in the second step is linearly polarized light, the laser frequency is 500-800kHz, the laser wavelength is 1064nm, and the pulse width is 7-30 ns.
The duration time of the laser pulse in the step two is 0.8-2ms, and the laser energy density is 0.21-0.27J/cm2
And in the second step, the maximum single pulse energy of the laser is 0.05J, and the diameter of the laser spot is 42 mu m.
The micro-nano multilayer structure comprises a micron-scale dimple-like structure and a nano-scale concentric ring-shaped structure.
When the multi-point array micro-nano multilayer structure on the surface of the amorphous carbon is prepared, the distance between two adjacent laser irradiation points is 10-30 mu m.
The invention has the beneficial effects that:
(1) the invention adopts nanosecond laser for processing, has low processing cost, high efficiency and simple processing mode, and is convenient for wide application.
(2) The micro-nano multilayer structure prepared on the surface of the amorphous carbon by the method comprises a micron-scale dimple-like structure and a nano-scale concentric ring-shaped structure, and the formed micro-nano multilayer structure is regular and uniform.
(3) The invention can form patterns with different patterns by changing the spacing.
(4) The invention has no toxicity and pollution, good stability and no need of vacuum environment.
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 application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention.
FIG. 1 is a flow chart of nanosecond laser induced amorphous carbon experiment and micro-nano multilayer structure images of the invention;
FIG. 2 is a three-dimensional optical image of a nanosecond laser-induced single-point micro-nano multilayer structure on the surface of amorphous carbon according to the invention;
FIG. 3 is SEM images of a nanosecond laser induced amorphous carbon surface single-point micro-nano multilayer structure under different pulse times;
FIG. 4 is an SEM image of a nanosecond laser induced multipoint array micro-nano multilayer structure on the surface of amorphous carbon;
fig. 5 is a three-dimensional optical image of a nanosecond laser-induced multipoint array micro-nano multilayer structure on the surface of amorphous carbon.
Detailed Description
The details of the present invention and its embodiments are further described below with reference to the accompanying drawings, but the present invention is not limited thereto, and the experimental methods are conventional unless otherwise specified, and the materials and reagents may be obtained from common sources unless otherwise specified. Referring to fig. 1 to 5, in the method for forming a micro-nano multilayer structure on an amorphous carbon surface by nanosecond laser irradiation, the point irradiation is performed on the amorphous carbon surface in the air by controlling the irradiation time and energy density of nanosecond laser pulses, and the micro-nano multilayer structure is prepared on the amorphous carbon surface by using the material removal effect of laser and the interference effect of light, and the method comprises the following steps:
step one, carrying out ultrasonic cleaning and drying on the polished amorphous carbon sample by using absolute ethyl alcohol to obtain a pretreated amorphous carbon sample;
step two, performing light path conversion and focusing on laser generated by the nanosecond fiber laser through a galvanometer system, and then vertically irradiating the laser on the surface of the amorphous carbon sample obtained in the step one; by controlling the irradiation time and energy density of nanosecond laser pulse, the micro-nano multilayer structure is prepared on the surface of amorphous carbon by utilizing the material removal effect of laser and the interference effect of light.
Further, in the step one, the cleaning temperature of ultrasonic cleaning is 50-60 ℃, the cleaning time is 4-6min, and the cleaning is naturally dried in the air.
Further, in the second step, the laser is linearly polarized light, the laser frequency is 500-800kHz, the laser wavelength is 1064nm, and the pulse width is 7-30 ns. The laser pulse duration is 0.8-2ms, and the laser energy density is 0.21-0.27J/cm2. The maximum single pulse energy of the laser is 0.05J, the diameter of a laser spot is 42 mu m, and the distance between two adjacent laser irradiation points is 10-30 mu m. The parameters such as laser frequency, pulse width, irradiation time, laser energy density, multi-point array spacing and the like can be conveniently adjusted through computer software; the experiment was performed in room temperature air.
Example 1:
the method for forming the micro-nano multilayer structure on the surface of the amorphous carbon by nanosecond laser irradiation induction comprises the following specific steps:
firstly, polishing an amorphous carbon sample with the diameter of 40mm and the thickness of 10mm, and carrying out ultrasonic cleaning and drying by using absolute ethyl alcohol to obtain a pretreated amorphous carbon sample. Wherein the cleaning temperature is 50 ℃, and the single cleaning time is 5 min.
Step two, performing light path conversion and focusing on laser generated by the nanosecond fiber laser through a galvanometer system, and then vertically irradiating the laser on the surface of the amorphous carbon sample obtained in the step one; by controlling the irradiation time and energy density of nanosecond laser pulse, the micro-nano multilayer structure is prepared on the surface of amorphous carbon by utilizing the material removal effect of laser and the interference effect of light. Wherein the laser processing parameters are that the laser frequency is 700kHz, the pulse width is 7ns, the laser pulse duration is 1ms, and the laser energy density is 0.235J/cm2
In the surface single-point micro-nano multilayer structure prepared in this embodiment, the micro-nano multilayer structure includes a micro-scale dimple-like structure and a nano-scale concentric ring-like structure, as shown in fig. 1 and 2, the surface of the surrounding material is not damaged. Wherein the diameter of the micron-scale dimple-like structure is 23.5 mu m, the depth is 7.65 mu m, and the period of the nanoscale concentric ring-like structure is about 550 nm.
As shown in fig. 3, SEM images of the laser pulse duration in the range of 0.4-2ms are observed, and the micro-nano multilayer structure in the portion (c) in fig. 3 is most regular and clear, and there are only a few residual particles around. When the laser pulse duration is less than or equal to 0.4ms, the nanoscale concentric ring structure cannot be generated, and when the laser pulse duration is greater than or equal to 1.2ms, the nanoscale concentric ring structure is damaged.
Example 2:
the method for forming the micro-nano multilayer structure on the surface of the amorphous carbon by nanosecond laser irradiation induction comprises the following specific steps:
firstly, polishing an amorphous carbon sample with the diameter of 40mm and the thickness of 10mm, and carrying out ultrasonic cleaning and drying by using absolute ethyl alcohol to obtain a pretreated amorphous carbon sample. Wherein the cleaning temperature is 50 ℃, and the single cleaning time is 5 min.
Step two, performing light path conversion and focusing on laser generated by a nanosecond fiber laser through a galvanometer system, then vertically irradiating the laser on the surface of the amorphous carbon sample obtained in the step one, and preparing a 5 × 5 multipoint array micro-nano multilayer structure by changing laser processing parameters, wherein the laser processing parameters comprise the laser frequency of 700kHz, the pulse width of 7ns, the laser pulse duration of 1ms and the laser energy density of 0.235J/cm2And the distance between two adjacent laser irradiation points is 20 mu m.
The micro-nano multilayer array structure prepared in the embodiment is shown in fig. 4 and 5, wherein the array structure is regular and well-arranged, and the single-point micro-nano multilayer structure has good retentivity, which indicates that the invention can be applied in a large area.
According to experimental results, the method provided by the invention can be used for preparing the micro-nano multilayer structure on the surface of the amorphous carbon by irradiating the surface of the amorphous carbon with nanosecond laser, and the generated structure can be prepared in a large area. The method is simple and efficient, the formed surface microstructure is regular and well-arranged, a feasible method is provided for efficiently preparing the amorphous carbon surface micro-nano multilayer structure in a large area, and the method has wide application prospects in the fields of mold forming, surface wettability, optical characteristics, catalytic characteristic adjustment and the like.
The above description is only a preferred example of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like of the present invention shall be included in the protection scope of the present invention.

Claims (7)

1. A method for forming a micro-nano multilayer structure on the surface of amorphous carbon by nanosecond laser irradiation is characterized by comprising the following steps: the method comprises the following steps of performing point irradiation on the surface of amorphous carbon in the air by controlling the irradiation time and energy density of nanosecond laser pulses, and preparing a micro-nano multilayer structure on the surface of the amorphous carbon by utilizing the material removal effect of laser and the interference effect of light, wherein the method comprises the following steps:
step one, carrying out ultrasonic cleaning and drying on the polished amorphous carbon sample by using absolute ethyl alcohol to obtain a pretreated amorphous carbon sample;
step two, performing light path conversion and focusing on laser generated by the nanosecond fiber laser through a galvanometer system, and then vertically irradiating the laser on the surface of the amorphous carbon sample obtained in the step one; by controlling the irradiation time and energy density of nanosecond laser pulse, the micro-nano multilayer structure is prepared on the surface of amorphous carbon by utilizing the material removal effect of laser and the interference effect of light.
2. The method for forming the micro-nano multilayer structure on the surface of the amorphous carbon through nanosecond laser irradiation induction according to claim 1, wherein the method comprises the following steps: and the cleaning temperature of the ultrasonic cleaning in the step one is 50-60 ℃, the cleaning time is 4-6min, and the ultrasonic cleaning is naturally dried in the air.
3. The method for forming the micro-nano multilayer structure on the surface of the amorphous carbon through nanosecond laser irradiation induction according to claim 1, wherein the method comprises the following steps: the laser in the second step is linearly polarized light, the laser frequency is 500-800kHz, the laser wavelength is 1064nm, and the pulse width is 7-30 ns.
4. The method for forming the micro-nano multilayer structure on the surface of the amorphous carbon through nanosecond laser irradiation induction according to claim 1, wherein the method comprises the following steps: the duration time of the laser pulse in the step two is 0.8-2ms, and the laser energy density is 0.21-0.27J/cm2
5. The method for forming the micro-nano multilayer structure on the surface of the amorphous carbon through nanosecond laser irradiation induction according to claim 1, wherein the method comprises the following steps: and in the second step, the maximum single pulse energy of the laser is 0.05J, and the diameter of the laser spot is 42 mu m.
6. The method for forming the micro-nano multilayer structure on the surface of the amorphous carbon through nanosecond laser irradiation induction according to claim 1, wherein the method comprises the following steps: the micro-nano multilayer structure comprises a micron-scale dimple-like structure and a nano-scale concentric ring-shaped structure.
7. The method for forming the micro-nano multilayer structure on the surface of the amorphous carbon through nanosecond laser irradiation induction according to claim 1, wherein the method comprises the following steps: when the multi-point array micro-nano multilayer structure on the surface of the amorphous carbon is prepared, the distance between two adjacent laser irradiation points is 10-30 mu m.
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CN112692434A (en) * 2021-01-08 2021-04-23 吉林大学 Method for preparing amorphous alloy micro concave and convex structure by nanosecond laser irradiation
CN112894143A (en) * 2021-01-25 2021-06-04 北京理工大学 Method for regulating and controlling surface wettability of stainless steel based on femtosecond laser direct writing scanning
CN113070565A (en) * 2021-04-27 2021-07-06 吉林大学 Method for preparing large-area conical microstructure on surface of amorphous alloy by nanosecond laser irradiation
CN113146051A (en) * 2021-04-23 2021-07-23 吉林大学 High-flexibility preparation method of large-area microstructure on surface of amorphous alloy
CN113770668A (en) * 2021-10-13 2021-12-10 湖南大学 Method for preparing optical glass super-hydrophobic functional surface by utilizing hot press molding
CN114147363A (en) * 2021-12-07 2022-03-08 吉林大学 Laser-induced amorphous carbon surface micro-nano composite structure and peripheral defect repair method

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112692434A (en) * 2021-01-08 2021-04-23 吉林大学 Method for preparing amorphous alloy micro concave and convex structure by nanosecond laser irradiation
CN112692434B (en) * 2021-01-08 2021-09-28 吉林大学 Method for preparing amorphous alloy micro concave and convex structure by nanosecond laser irradiation
CN112894143A (en) * 2021-01-25 2021-06-04 北京理工大学 Method for regulating and controlling surface wettability of stainless steel based on femtosecond laser direct writing scanning
CN113146051A (en) * 2021-04-23 2021-07-23 吉林大学 High-flexibility preparation method of large-area microstructure on surface of amorphous alloy
CN113070565A (en) * 2021-04-27 2021-07-06 吉林大学 Method for preparing large-area conical microstructure on surface of amorphous alloy by nanosecond laser irradiation
CN113070565B (en) * 2021-04-27 2022-01-25 吉林大学 Method for preparing large-area conical microstructure on surface of amorphous alloy by nanosecond laser irradiation
CN113770668A (en) * 2021-10-13 2021-12-10 湖南大学 Method for preparing optical glass super-hydrophobic functional surface by utilizing hot press molding
CN114147363A (en) * 2021-12-07 2022-03-08 吉林大学 Laser-induced amorphous carbon surface micro-nano composite structure and peripheral defect repair method
CN114147363B (en) * 2021-12-07 2024-03-22 吉林大学 Laser-induced amorphous carbon surface micro-nano composite structure and peripheral defect repairing method

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