CN113182693A - Femtosecond laser preparation SiO2Method for swelling micro-nano structure on metal interface - Google Patents
Femtosecond laser preparation SiO2Method for swelling micro-nano structure on metal interface Download PDFInfo
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Abstract
Femtosecond laser preparation SiO2A method for swelling a micro-nano structure on a metal interface, which relates to the field of femtosecond laser micro-nano processing. The method adopts femtosecond laser direct writing technology to focus laser on SiO2And (glass) -metal film interface, ablating the metal film at the interface to form a convex micro-nano size structure. The energy of the pulse laser is controlled by using a neutral density attenuation sheet, a three-dimensional displacement table system is controlled by using a displacement table control program, the control of scanning speed and scanning distance is realized, and a parameter database of which the processing parameters correspond to the size of the swelling micro-nano structure is established.
Description
The technical field is as follows:
the invention relates to the field of femtosecond laser micro-nano processing, in particular to a method for preparing SiO by femtosecond laser direct writing2A method for swelling a micro-nano structure on a metal interface.
Background art:
the special micro-nano structure of the biological surface in nature causes the biological surface to show extraordinary surface performance. Such as: the colorful wings of many insects are structural colors exhibited by selective diffraction and reflection of light by the ordered micro-nano structure; the lotus leaves which are discharged with silt but not dyed are shown to be super-hydrophobic, and are formed by the papillary micron-sized coarse structure on the surfaces of the lotus leaves and the hydrophobic waxy covering layer; the gecko's sole with strong adsorption capacity shows super-water absorption due to the fact that a large number of micron-sized villi structures grow on the surface of gecko's toes, and nano-sized branch structures (secondary structures) are further arranged on the tips of the micron-sized villi. The extraordinary functions expressed by the surface micro-nano characteristic structures suggest that people prepare characteristic structures with certain rules (modes) on the surface of a material by a simulation manufacturing technology so as to realize various surface functions required by people. The processing and manufacturing of the micro mechanical parts with special surface functions are realized through the characteristic structure of micro-nano size, and the micro mechanical parts are applied to a plurality of future emerging industries, such as: the energy conversion device in biomedical sensing device, micro-fluidic device, new energy, aviation and military and other application fields have important strategic significance.
The processing method capable of realizing the surface micro-nano structure is mainly realized by physical vapor deposition, chemical etching, photoetching, nano-imprinting and ion beam processing, but the complex process for preparing the specific microstructure on the surface of the material and the high cost greatly limit the wide application of the micro-scale material in the actual production life. The femtosecond laser processing technology has unique advantages in the field of surface micro-nano structure processing due to the characteristics of high precision, good controllability, wide applicable materials and the like. In recent years, researchers have conducted a large number of micro-nano processing experiments on the surface of a metal thin film material by using femtosecond laser, and the micro-nano structure obtained by the experiments is unique in the fields of micro color printing, photoelectric sensing technology, color display technology and the like. However, in the femtosecond laser metal film experiment, a laser backward ablation method (directly focusing laser on the surface of the metal film) is mostly adopted, and a single-point single-pulse line-by-line scanning processing mode is used. The experimental method is generally used for preparing the convex array structure, and has poor processing effect and larger surface roughness.
The invention content is as follows:
against the background, the invention provides a method for focusing laser on SiO by adopting a laser forward ablation technology2Preparing SiO at the interface of the metal film by femtosecond laser direct writing technology2A method for swelling a micro-nano structure on a metal interface.
To achieve the above object, the processing method is as follows:
focusing laser on SiO by adopting laser forward ablation technology2Preparing SiO at the interface of the metal film by femtosecond laser direct writing technology2A method for swelling a micro-nano structure on a metal interface.
Preparation of SiO by so-called femtosecond laser2The method for expanding the micro-nano structure on the metal interface is characterized in that laser is focused on SiO by adopting a laser forward ablation technology2Preparing SiO at the interface of the metal film by femtosecond laser direct writing technology2-a method for swelling micro-nano structures at a metal interface;
adjusting process parameters in SiO2-forming an ablation structure at the interface of the metal film and forming a swelling (bulge) structure on the surface of the metal film; obtaining a processing parameter and a parameter rule of the swelling micro-nano structure; establishing femtosecond direct writing technology to prepare SiO2A database of corresponding processing parameters of the processing parameters and the dimensions of the micro-nano characteristic structure in the method for swelling the micro-nano structure on the metal interface.
The method specifically comprises the following steps:
(1) debugging a femtosecond laser processing system, wherein a beam of femtosecond laser is emitted by a femtosecond laser amplification system, enters a micro-processing system after passing through a continuously adjustable neutral density attenuation sheet, and is focused by an objective with the numerical aperture N.A. ═ 0.25 and the amplification rate of 10 times;
(2) SiO for experiment2-a metal film as a sample. Selecting SiO2The glass is used as a substrate material, has the advantages of good dimensional stability, low thermal expansion coefficient, high ablation threshold value and the like, and has good light transmission property, thereby facilitating laser focusing on an interface; in SiO2Preparing a metal film on one surface, preferably using vacuum thermal evaporation method to form a metal film on SiO2Surface-deposited metal film, SiO2The thickness of the substrate is 1-10 mm, the thickness of the metal film is 50-300 nm, and preferably, a silver film, a copper film, an aluminum film or two metals of the silver film, the copper film and the aluminum film form a double-layer metal film;
(3) placing the glass substrate plated with the metal film on a sample objective table for horizontal adjustment, attaching the metal film surface downwards to the sample objective table, introducing the parameter-adjusted femtosecond laser into a micro-processing system, and scanning the micro-processing system by passing through the glass substrate from the surface of the glass substrate to focus on the interface of the glass and the metal film (preferably by passing through the glass substrate by a micro-processing objective lens with the numerical aperture N.A. of 0.25 to focus on the interface of the glass and the metal film); the focusing position and the focusing condition of the sample are observed by the CCD in real time;
(4) the control of pulse laser energy is realized by utilizing a neutral density attenuation sheet, a three-dimensional displacement table system is controlled by a displacement table control program, the control of scanning speed and scanning distance is realized, and a structural rule of which the processing parameters correspond to the swelling micro-nano structure is obtained; and establishing a processing parameter database of the micro-nano characteristic structure prepared by the method.
The principle of the invention is as follows:
femtosecond laser through SiO2When the metal film is irradiated on the surface of the metal film, the surface electrons of the metal instantly absorb laser (photon) energy, but due to the limited domain effect of the interface on the electron movement, the laser energy absorbed by the electrons (through electron-electron collision) is almost completely converted into electron heat energy, so that extremely high thermal pressure is generated, and when the thermal pressure is greater than that of the metal film and SiO2The bonding force between the surfaces, the metal film, when impacted, creates a structure that bulges away from the outward surface of the glass, i.e., an interface "popped" structure.
Compared with the prior art, the invention has the following advantages:
1. provides a method for focusing laser on SiO by adopting a laser forward ablation technology2-a metal film interface, the raised structures being prepared in a direct scanning manner;
2. preparing a formed convex structure, wherein the convex structure on the surface of the formed convex structure is smooth and has no other microstructures;
3. the experiment adopts a femtosecond laser direct writing mode, utilizes a neutral density attenuation sheet to control laser energy, utilizes a control program to control a three-dimensional displacement table system, and can realize large-area processing in a short time.
Description of the drawings:
FIG. 1 is a diagram showing an optical path structure of a device part of the present invention.
The main symbols are as follows:
1. femtosecond laser regeneration amplification system 2, attenuation sheet 3 and semi-transparent semi-reflecting mirror
4. Focusing mirror 5, sample 6 and three-dimensional sample stage
7. CCD camera 8, computer control end
FIG. 2 is a schematic view of laser focusing sample processing in the present invention. Left: laser focusing sample processing schematic front view; and (3) right: a top view of the path.
FIG. 3 is based on Ag-SiO2And preparing a structural morphology graph by adopting a laser forward ablation technology. (a) SiO 22An Ag film interface micrograph, (b) an Ag film surface SEM image, (c) a grating height, and (d) an Ag film surface three-dimensional morphology image.
FIG. 4 is based on Cu-SiO2: and a raised grating structure on the Cu film surface. (a) SEM picture, (b) three-dimensional topography, and (c) grating height.
FIG. 5 is a Cu-Ag-SiO-based2: and a raised grating structure with a Cu surface. (a) SEM picture, (b) three-dimensional topography, and (c) grating height.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to the accompanying fig. 1 and examples, but the present invention is not limited to the examples.
1. Placing a glass sheet (5) plated with a metal film on a sample objective table (6);
specifically, the glass substrate plated with the metal film is placed on a sample stage to be horizontally adjusted, and the metal film surface is attached to the sample stage. Wherein the glass substrate has a thickness of 5mm, and the metal film is selected from Ag and Cu films with a thickness of 200nm and Cu-Ag double-layer films (corresponding sequence is Cu-Ag-SiO)2Cu and Ag are each 100nm thick), and the three-dimensional stage system is operated by the stage control program.
2. Debugging a femtosecond laser processing system;
specifically, one beam of femtosecond laser is emitted from a femtosecond laser amplification system (1), passes through a continuously adjustable neutral density attenuation sheet (2), enters an OLYPUS micromachining system, and is finally focused through an objective lens (4) with the numerical aperture N.A. of 0.25 and the magnification of 10 times.
3. Focusing laser on the glass-metal film interface;
specifically, the laser is focused on the glass-metal film interface (see fig. 2), and the focusing position and focusing condition of the sample are observed by the CCD (7) in real time.
4. Preparing a swelling micro-nano grating structure by femtosecond laser direct writing;
specifically, the laser energy is controlled by a continuously adjustable neutral density attenuation sheet. The preparation of a large-area micro-nano structure is realized through the movement of the displacement table, and a three-dimensional displacement table system is controlled by utilizing a displacement table control program, so that the control of the scanning speed and the scanning distance is realized.
5. Summarizing parameterization rules of processing parameters and structural morphology;
specifically, a series of micro-nano structures are prepared by utilizing processing parameters such as different laser fluxes, scanning speeds and the like, and are characterized. And researching the relation between different processing parameters and the prepared swelling structure morphology, and establishing a processing parameter database of the micro-nano characteristic structure prepared by the method.
As a result, it was found that: and forming an ablation structure at the interface of the glass-metal film and forming a raised grating structure on the surface of the metal film by specific processing parameters. And obtaining the parameterization rule of the laser flux, the scanning speed and the height of the convex grating structure. And the height of the convex grating is gradually increased along with the increase of the laser flux until the grating is broken; along with the increase of the scanning speed, the height of the raised grating is gradually reduced, and the phenomenon of uneven height of the raised grating is gradually obvious.
6. Structural appearances of different metal films;
the metal film is Ag film with thickness of 200 nm. The laser flux is 0.247J/cm2The scanning speed is 1mm/s, the grating period is 20 μm, and the height of the obtained convex grating is 0.251 μm, see fig. 3.
The metal film is a Cu film with the thickness of 200 nm. The laser flux is 0.0707J/cm2The scanning speed is 1mm/s, the grating period is 20 μm, and the obtained raised grating height is 0.414 μm, see fig. 4.
The metal film is a Cu-Ag double-layer film (the corresponding sequence is Cu-Ag-SiO)2Cu and Ag are each 100nm thick), and the laser flux is 0.177J/cm2The scanning speed is 1mm/s, the grating period is 20 μm, and the height of the obtained raised grating is 0.097 μm, see fig. 5.
The invention provides a special processing method, which adopts a laser forward ablation technology to focus laser on SiO2Preparing SiO at the interface of the metal film by femtosecond laser direct writing technology2-a metal interface expanded micro-nano grating structure.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. Femtosecond laser preparation SiO2-method for swelling micro-nano structures at metal interfaces, characterized in that laser is focused on SiO2Preparing SiO at the interface of the metal film by femtosecond laser direct writing technology2-a method of swelling micro-nano sized structures at a metal interface; adjusting process parameters in SiO2The interface of the metal film forms an ablation structure and a raised structure on the surface of the metal film.
2. The femtosecond laser prepared SiO according to claim 12-method for swelling micro-nano structures at a metal interface, characterized in that a femtosecond laser passes through the SiO2When the metal film is irradiated on the surface of the metal film, the surface electrons of the metal instantly absorb laser (photon) energy, but due to the limited domain effect of the interface on the electron movement, the laser energy absorbed by the electrons (through electron-electron collision) is almost completely converted into electron heat energy, so that extremely high thermal pressure is generated, and when the thermal pressure is greater than that of the metal film and SiO2The metal film generates back SiO after being impacted during the bonding force between the surfaces2The outward surface of (a) is convex, i.e., the interfacial "puff.
3. The femtosecond laser prepared SiO according to claim 12The method for swelling the micro-nano structure on the metal interface is characterized by comprising the following steps
(1) Debugging a femtosecond laser processing system, enabling one beam of femtosecond laser to enter a micro-processing system after passing through a continuously adjustable neutral density attenuation sheet, and finally focusing the laser by an objective with the numerical aperture N.A. ═ 0.25 and the magnification of 10 times;
(2) SiO for experiment2-a metal film as a sample; selecting SiO2(glass) as substrate material in SiO2Preparing a metal film on one side surface, preferably using vacuum thermal evaporation method to form SiO2Evaporating a metal film on the surface;
(3) placing the glass substrate plated with the metal film on a sample objective table for horizontal adjustment, attaching the metal film with the surface facing downwards to the sample objective table, introducing the parameter-adjusted femtosecond laser into a micro-processing system, passing through the glass substrate from the surface of the glass substrate, focusing to the interface between the glass and the metal film, and scanning to obtain SiO2-a metallic interface expanded micro-nano structure; the focusing position and the focusing condition of the sample are observed by the CCD in real time;
(4) the control of pulse laser energy is realized by utilizing a neutral density attenuation sheet, the control of scanning speed and scanning distance is realized by controlling a three-dimensional displacement platform system through a control program, and a parameter database of which the processing parameters correspond to the sizes of the swelling micro-nano structures is obtained.
4. The femtosecond laser prepared SiO according to claim 32The method for swelling the micro-nano structure on the metal interface is characterized in that the sample stage is a three-dimensional motion stage, and the motion speed and the moving distance of the sample stage are controlled by a programmed computer program.
5. The femtosecond laser prepared SiO according to claim 32-method for swelling micro-nano structure on metal interface, characterized in that the SiO2The thickness of the (glass) substrate is 1-10 mm, and the thickness of the metal filmThe degree is 50nm to 300nm, and the silver, copper, aluminum film or two metals thereof are preferably formed into a double-layer metal film.
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