CN111185678A - Method for preparing hollow structure on surface and inside of transparent material - Google Patents
Method for preparing hollow structure on surface and inside of transparent material Download PDFInfo
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- CN111185678A CN111185678A CN202010082069.9A CN202010082069A CN111185678A CN 111185678 A CN111185678 A CN 111185678A CN 202010082069 A CN202010082069 A CN 202010082069A CN 111185678 A CN111185678 A CN 111185678A
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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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- 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
- B08B3/02—Cleaning by the force of jets or sprays
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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
- 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
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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
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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
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
Abstract
The invention discloses a method for preparing hollow structures on the surface and inside of a transparent material, which belongs to the technical field of femtosecond laser micro-nano processing. The method can realize high-efficiency and high-precision processing of various common transparent materials in a vacuum-free environment, and solves the problems of high environmental requirement and low processing efficiency in the prior art.
Description
Technical Field
The invention belongs to the technical field of femtosecond laser micro-nano processing, and particularly relates to a method for directly writing a hundred-nanometer-precision uniform line structure in a transparent material by using femtosecond laser, and preparing a hollow structure with ultrahigh processing precision and any depth-diameter ratio on the surface and the inside by subsequent polishing and wet etching processes.
Background
With the continuous progress of scientific technology, people have higher and higher requirements on integration and miniaturization, and compared with a large-size device with the same function, the device prepared by using the micro-nano structure has the advantages of low energy consumption, high efficiency, high sensitivity and the like, and is convenient for multifunctional integration due to small volume. The same is true for the optical field. In recent years, a photoetching process is generally used for preparing a micro-nano optical component with a structure size lower than a wavelength. A reticle is generally required to transfer a pattern to a substrate whose surface is coated with a photosensitive resin, and then patterning of the material surface is achieved by means of development and secondary dry etching. This approach typically requires multiple steps and different reticles for different patterns. In addition, these optical lithography processes typically only enable the fabrication of quasi-three-dimensional structures and require a strict vacuum environment, further limiting their application.
Although the common femtosecond laser direct writing technology can realize the processing of any three-dimensional structure with the precision of hundreds of nanometers on a polymer material, the processing of a subsequent structure can be influenced by the scraps caused by direct ablation on the surface of a hard and brittle material, and the thickness of an internal processing optical device is larger due to the fact that the refractive index change amount of a modified area is smaller in internal processing. In addition, the laser is usually used to directly induce the periodic grating structure on the surface and the inner processing area, which affects the precision and controllability of the processing.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problems to be solved by the invention are as follows: provides a processing method for preparing a hollow structure on the surface and inside of a transparent material. Through accurate control polarization and processing power, a femtosecond laser direct writing mode is used for directly writing a modified area with the precision of hundreds of nanometers in a transparent material, then a mechanical/ion beam thinning mode is used for thinning the surface of the transparent material to a processing area position (surface processing), finally a wet etching process is used for etching the material, and finally the preparation of the hollow structure with the precision of hundreds of nanometers and with a high-precision arbitrarily-designed structure is realized. The method can realize high-efficiency and high-precision processing of various common transparent materials in a vacuum-free environment, and solves the problems of high environmental requirement and low processing efficiency in the prior art.
The invention is realized by the following technical scheme:
a method for preparing a hollow structure on the surface and inside of a transparent material comprises the following specific steps:
the method comprises the following steps: leveling a sample;
firstly, fixing a sample to be processed on the surface of a displacement platform with a biaxial adjusting device, then adjusting the power of a laser to be lower than the damage threshold of a material (when focusing, a focused light spot can be seen under a CCD), opening a laser light gate, and focusing the laser on the surface of the sample by adjusting the height of the displacement platform; then, repeatedly moving the displacement platform for 5cm along the vertical direction, and ensuring that the focus is always on the surface of the sample through a two-axis adjusting device; finally, repeatedly moving the displacement platform for 5cm along the horizontal direction, and ensuring that the focus is always on the surface of the sample through a two-axis adjusting device; at this time, the leveling of the sample to be processed is finished;
step two, the femtosecond laser writes a modified structure in the material;
the method comprises the following specific steps: laser emitted by the laser passes through a Spatial Light Modulator (SLM) and then is subjected to phase modulation, (wherein the SLM is used for loading a holographic phase diagram corrected based on spherical aberration with mismatched refractive index so as to ensure the length uniformity of structures with different depths in the processing process), and then sequentially passes through a first convex lens L1And a second convex lens L2The 4f system is formed by projecting the phase distribution on the spatial light modulator to the position of an objective lens entrance pupil and then focusing the phase distribution in the transparent material through the objective lens for processing; in the process of writing the structure internally, a point-by-point scanning mode is used and startsThe polarization of the laser is kept to be perpendicular to the processing trace, so that the processing of the internal single line structure is realized; in addition, in order to facilitate observation in the subsequent polishing step, a plurality of nanowire arrays are inscribed at different depths of the cross section of the sample to be used as marks;
step three, removing the surface layer of the sample (for surface structure);
the method comprises the following specific steps: firstly, roughly polishing a processed sample by using abrasive paper with a small mesh number, quickly thinning the sample, and finely polishing the sample by using the abrasive paper with a large mesh number when the processing trace of the sample is close to the surface of the sample under the observation of a microscope; secondarily observing the depth position of the marked section of the polished sample by using a microscope; finally, polishing the sample by using polishing powder for final ultra-fine polishing, and polishing the sample to the surface right to expose a processing trace through repeated polishing and microscope observation for multiple times;
step four, anisotropic etching;
and proportioning the wet etching solution, putting the polished sample into the wet etching solution for ultrasonic wet etching, taking out the sample, respectively washing with ethanol and deionized water, and blow-drying with an aurilave to obtain the required surface hyperfine structure.
Further, the sample to be processed in the step one is a common transparent hard and brittle material: such as fused silica, sapphire, YAG crystal, etc., and may have a thickness of 100 μm to 1 mm; the adjusting device is a leveling device with two knobs, and can adjust the pitching and rolling angles of the sample table respectively; fixing a sample on a glass slide by using double faced adhesive tape, fixing the glass slide on a sample table by using a holding device, and downwards mounting a cover glass on a mirror bracket with a clamp; the moving platform is formed by combining a nano piezoelectric platform and a stepping motor platform, wherein the stroke of the piezoelectric platform is 200 multiplied by 200 mu m; the stroke of the stepping motor is 20x20 mm.
Further, the spherical aberration correction depth range of the second step is 10 μm-2mm, and the laser processing depth is 20 μm-1 mm; the femtosecond laser wavelength used in processing is 515nm, 800nm or 1030nm, and the single pulse energy is 50nJ-1000nJ according to the selected objective lens; the numerical aperture of the objective lens used in the processing is 0.5-0.9; the point interval of the processing line structure is 10nm-2000 n; the interval between lines is 400nm-5000 nm; the direction and polarization direction of the scanning structure is 0-180 deg..
Further, the surface of the sample material in the third step is polished by using rough polishing sand paper of 400#, 1000# and 3000#, and fine polishing sand paper of 5000# and 7000 #; the polishing powder for ultra-fine polishing is 12000#, and the polishing speed is 30-150 r/min.
Further, the wet etching process described in the fourth step uses different etching solutions to perform anisotropic wet etching for different materials according to their chemical properties, such as 20% by volume of HF for quartz and sapphire, and 40% by volume of H for YAG crystal3PO4。
Compared with the prior art, the invention has the following advantages:
(1) compared with the traditional photoetching process, the method does not need a vacuum environment, can realize random patterning ultrahigh-precision processing, and can realize the capability of three-dimensional processing;
(2) compared with femtosecond laser direct writing, the mode overcomes the limitation that the prior surface and internal processing can only process the stripe structure with fixed period and the surface ablation coarse structure, and realizes the processing precision of hundreds of nanometers;
(3) the invention can be applied to the field of fine processing of various hard and brittle materials in terms of expansibility, and has wide application prospects in the fields of micro-nano optics, micro-fluidics, micro-machinery and the like.
Drawings
FIG. 1 is a schematic diagram of the optical path of a method for preparing a hollow structure on the surface and inside of a transparent material according to the present invention, wherein L1、L2And L3Is a plano-convex lens, the SLM is a liquid crystal spatial light modulator, M1And M2Is a total reflection mirror, a CCD-camera;
FIG. 2 is a flow chart of a method for preparing an ultra-high precision structure on the surface and inside of a transparent hard and brittle material for preparing a hollow structure on the surface and inside of the transparent material according to the invention;
FIG. 3 is a hollow array of nanowires in different directions obtained on the surface of fused quartz by the method for preparing a hollow structure on the surface and inside of a transparent hard and brittle material, and preparing an ultra-high precision structure on the surface and inside of the transparent hard and brittle material according to the invention; wherein the line interval is 400nm, and the angles are 0 degree (a), 45 degree (b), 90 degree (c) and 135 degree (d), respectively.
FIG. 4 is a nanowire array with a duty ratio of 50% obtained on the surface of fused quartz by a method for preparing a hollow structure on the surface and inside of a transparent material and preparing an ultra-high precision structure on the surface and inside of a transparent hard and brittle material according to the present invention;
FIG. 5 shows a nanowire array with a width of 100nm and a direction of 45 obtained on the surface of YAG crystal by the method for preparing the hollow structure on the surface and inside of the transparent material.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Quartz surface processing high-precision nano line array structure
The method comprises the steps of utilizing femtosecond laser to write a uniform line structure in quartz, then using mechanical polishing to polish a sample to the vicinity of a processing area, and then using a wet etching process to perform anisotropic etching, thereby realizing a uniform nanowire array structure on the surface of the quartz.
A method for preparing an ultrahigh-precision structure on the surface of a transparent hard and brittle material comprises the following specific steps:
(1) preparing and leveling a sample;
first, a large fused silica sample having a thickness of 500 μm was cut into 20X20mm pieces by a glass cutter2Respectively placing into test tubes containing acetone and alcohol, performing ultrasonic treatment for 20min, finally placing into a beaker containing deionized water, performing ultrasonic treatment for 10min, and drying with nitrogen. The quartz sample was then mounted to a glass slide using double sided tape and the slide was placed on the displacement stage of the laser processing system. Mounting ofThe upper numerical aperture is 0.9, the magnification is 100 multiplied by the Orlynbas objective lens, the laser single pulse energy is adjusted to 5nJ, the diaphragm is opened, and the laser is just focused on the interface of air and quartz by adjusting the height of the displacement platform. Repeatedly moving for 5cm along the vertical direction and the horizontal direction respectively, and adjusting two knobs of the adjusting platform after moving to ensure that the focus is always focused on the interface of air and quartz before and after moving; finally, through multiple cycles of adjustment, when the displacement platform moves, the focus of the displacement platform is always focused at the interface of air and quartz, and the displacement platform is leveled at the moment.
(2) Etching and processing the uniform structure in the quartz;
first, the pulse energy of the laser was adjusted to 200nJ by the control software, the spherical aberration correction phase was loaded on the SLM, and the focal position was moved to the interface between air and quartz using the piezoelectric stage. The piezoelectric stage was then moved down 50 μm, at which time the focal point of the laser was focused inside the sample. A piezo-electric stage machining program was introduced, here using a linear array machining program with angles of 0 degrees, 45 degrees, 90 degrees and 135 degrees, with a dot spacing of 50nm and a line spacing of 400 nm. And in the process of internal processing, controlling the polarization direction of the laser to be vertical to the scanning direction in real time through a processing program until the processing is finished.
And then, taking down the glass slide fixed on the sample table, taking down the processed quartz sample from the glass slide, respectively putting the quartz sample into acetone and alcohol solution for ultrasonic treatment for 10min, and finally drying the quartz sample by using nitrogen.
(3) Mechanical thinning treatment of the surface of the sample;
the processed sample is horizontally embedded into polymer resin by using a cold embedding mode, sand papers with the mesh numbers of 500#, 1000# and 3000# are respectively used for rough polishing, and whether the position of the inscribed structure in the sample is close to the surface or not is observed by using a microscope. If the internal structure is close to the surface, the sandpaper is changed into 5000# and 7000# for fine polishing to remove the rough scratches on the surface, the position of the structure is repeatedly observed using a microscope, and when the structure is on the surface, the sample is mechanically polished using cerium oxide polishing powder at a polishing speed of 70r/min for 20 min. The polished sample was then placed in acetone to remove the polymer resin.
(3) A surface wet etching process of the sample;
preparing 10mL of HF solution with the volume fraction ratio of 2%, placing the sample with the thinned and polished surface into the solution for ultrasonic treatment for 400s, taking out the sample, washing the sample with ethanol and deionized water for 2min, and finally blowing the sample with nitrogen.
Example 2
YAG crystal surface 45-degree direction nanowire array structure
The method comprises the steps of utilizing femtosecond laser to write a modified structure with uniform nanometer precision in a YAG crystal, utilizing an ion beam thinning instrument to carry out quantitative thickness thinning on the surface of the YAG crystal, and finally utilizing a wet etching process to carry out anisotropic etching on the YAG.
(1) Leveling of a sample table:
as in example 1.
(2) Writing of YAG internal uniform nano structure
The only difference from example 1 is the loading of the spatial light modulator with different spherical aberration correction holograms and the single pulse energy used. The single pulse energy used here was 247nJ with an internal depth of 30 um.
(3) Focused ion beam thinning
And flatly pasting the prepared YAG sample on an aluminum column of an ion beam thinning instrument by using a quick-drying adhesive, putting the aluminum column into the ion beam thinning instrument, adjusting the voltage to be 6kV, and keeping the time for 3 hours, wherein the ion beam thinning instrument can thin the sample by 30 um. And taking out the thinned aluminum column, and washing the quick-drying glue by using an ethanol solution to obtain the thinned YAG crystal material.
(4) And (3) wet etching process of the sample surface:
preparing H with the volume fraction ratio of 40%3PO410mL of solution, placing the sample with the thinned and polished surface into a sealed container containing etching solution, placing the container into an oven with the temperature of 90 ℃ for 3 hours to carry out anisotropic etching, then taking out the container, and flushing the container by using ethanol and deionized waterWashing for 2min, and finally blowing by using nitrogen.
It can be seen from fig. 2 that structures with arbitrary depth and three-dimensional arrangement can be inscribed inside by using femtosecond laser, and the length and the interval of the structures are limited by the displacement platform.
As can be seen from FIG. 3, the method of the present invention can be used to prepare hollow nanowire arrays with any direction and period.
As can be seen from fig. 4, the hollow nanowire array structure with different duty ratios can be realized by using the method of the present invention.
As can be seen from FIG. 5, the method of the present invention can realize high-precision hollow nanowire structures on the surfaces and inside of different materials.
Claims (4)
1. A method for preparing a hollow structure on the surface and inside of a transparent material is characterized by comprising the following specific steps:
the method comprises the following steps: leveling a sample;
firstly, fixing a sample to be processed on the surface of a displacement platform with a two-axis adjusting device, then turning on a laser light gate by the power of a laser, and focusing the laser on the surface of the sample by adjusting the height of the displacement platform; then, repeatedly moving the displacement platform for 5cm along the vertical direction, and ensuring that the focus is always on the surface of the sample through a two-axis adjusting device; finally, repeatedly moving the displacement platform for 5cm along the horizontal direction, and ensuring that the focus is always on the surface of the sample through a two-axis adjusting device; at this time, the leveling of the sample to be processed is finished;
step two, the femtosecond laser writes a modified structure in the material;
the method comprises the following specific steps: laser emitted by the laser passes through a Spatial Light Modulator (SLM) and then is subjected to phase modulation, and then sequentially passes through a first convex lens L1And a second convex lens L2The 4f system is formed by projecting the phase distribution on the spatial light modulator to the position of an objective lens entrance pupil and then focusing the phase distribution in the transparent material through the objective lens for processing; in the process of writing the structure inside, a point-by-point scanning mode is used, and the polarization of laser is always kept perpendicular to the processing trace, so that the processing of the single line structure inside is realized; in addition, it is characterized by thatThe subsequent polishing step is convenient to observe, and a plurality of nanowire arrays are inscribed at different depths of the cross section of the sample to be used as marks;
step three, removing the surface layer of the sample:
the method comprises the following specific steps: firstly, roughly polishing a processed sample by using abrasive paper with a small mesh number, quickly thinning the sample, and finely polishing the sample by using the abrasive paper with a large mesh number when the processing trace of the sample is close to the surface of the sample under the observation of a microscope; secondarily observing the depth position of the marked section of the polished sample by using a microscope; finally, polishing the sample by using polishing powder for final ultra-fine polishing, and polishing the sample to the surface right to expose a processing trace through repeated polishing and microscope observation for multiple times;
step four, anisotropic etching;
and proportioning the wet etching solution, putting the polished sample into the wet etching solution for ultrasonic wet etching, taking out the sample, respectively washing with ethanol and deionized water, and blow-drying with an aurilave to obtain the required surface hyperfine structure.
2. The method for preparing the hollow structure on the surface and the inside of the transparent material according to claim 1, wherein the sample to be processed is a common transparent hard and brittle material in the step one: such as fused silica, sapphire, YAG crystal, etc., and may have a thickness of 100 μm to 1 mm; the adjusting device is a leveling device with two knobs, and can adjust the pitching and rolling angles of the sample table respectively; fixing a sample on a glass slide by using double faced adhesive tape, fixing the glass slide on a sample table by using a holding device, and downwards mounting a cover glass on a mirror bracket with a clamp; the moving platform is formed by combining a nano piezoelectric platform and a stepping motor platform, wherein the stroke of the piezoelectric platform is 200 multiplied by 200 mu m; the stroke of the stepping motor is 20x20 mm.
3. The method for preparing the hollow structure on the surface and the interior of the transparent material according to claim 1, wherein the spherical aberration correction depth range in the second step is 10 μm to 2mm, and the laser processing depth is 20 μm to 1 mm; the femtosecond laser wavelength used in processing is 515nm, 800nm or 1030nm, and the single pulse energy is 50nJ-1000nJ according to the selected objective lens; the numerical aperture of the objective lens used in the processing is 0.5-0.9; the point interval of the processing line structure is 10nm-2000 n; the interval between lines is 400nm-5000 nm; the direction and polarization direction of the scanning structure is 0-180 deg..
4. The method for preparing the hollow structures on the surface and the inside of the transparent material according to claim 1, wherein the surface polishing of the sample material in the third step uses rough polishing sand paper with 400#, 1000# and 3000#, and the fine polishing uses sand paper with 5000# and 7000 #; the polishing powder for ultra-fine polishing is 12000#, and the polishing speed is 30-150 r/min.
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| CN113478088A (en) * | 2021-06-29 | 2021-10-08 | 杭州电子科技大学 | Method for improving roughness of inner surface of laser ablation micropore and groove |
| CN114888443A (en) * | 2022-03-30 | 2022-08-12 | 北京理工大学 | Method for high-dimensional precision engraving on two sides of transparent material by femtosecond laser |
| CN114952020A (en) * | 2022-06-15 | 2022-08-30 | 吉林大学 | High-efficiency processing method for high-aspect-ratio nano structure of hard and brittle material |
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