CN112192325B - Method for machining micro-nano scale through hole in transparent hard and brittle material by femtosecond laser - Google Patents
Method for machining micro-nano scale through hole in transparent hard and brittle material by femtosecond laser Download PDFInfo
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- CN112192325B CN112192325B CN202011072075.2A CN202011072075A CN112192325B CN 112192325 B CN112192325 B CN 112192325B CN 202011072075 A CN202011072075 A CN 202011072075A CN 112192325 B CN112192325 B CN 112192325B
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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
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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
- B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
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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
- B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
- B23K26/0648—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms comprising lenses
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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
- B23K26/38—Removing material by boring or cutting
- B23K26/382—Removing material by boring or cutting by boring
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
Abstract
The invention relates to a method for processing a micro-nano scale through hole on a transparent hard and brittle material by femtosecond laser, belonging to the technical field of laser application. The invention aims to solve the problems of high cost and low efficiency in micro-nano scale through hole processing in the existing method. According to the method, femtosecond laser space is integrated into a Bessel beam, the size of a modified hole formed in a transparent hard and brittle material can be continuously adjusted by controlling the diameter of the Bessel beam, modified hole array processing is realized by combining the movement of a translation table, a blind hole array is formed by wet etching, and finally, redundant materials are removed by grinding and polishing through a grinding and polishing machine to form a micro-nano-scale through hole. The micro-nano through hole processed by the method has the advantages of adjustable outlet size, capability of processing large-area arrays, short single-hole processing time, high processing efficiency and low cost, and can be applied to the fields of cell screening, DNA molecular sequencing and the like.
Description
Technical Field
The invention relates to a method for processing a micro-nano scale through hole on a transparent hard and brittle material by femtosecond laser, belonging to the technical field of laser application.
Background
The micro-nano scale through hole is a common structure and is widely applied to the fields of aviation, biology, chemical industry, new energy and the like. Taking the biological field as an example, the micro-through hole can realize the screening of target cells, and the nano-through hole can realize molecular screening or DNA sequencing by means of electrophoresis driving. However, the strength and limited stability of micro-nano-scale through holes have become major obstacles for biochemical nanopore research. The transparent hard and brittle material glass has the characteristics of good wear resistance, high strength, good light transmittance and the like, and the problems of insufficient strength and stability under the condition of large flow can be effectively solved by processing the micro-nano through holes by using the glass. For the micro-nano through holes of hard and brittle materials such as glass, sapphire and the like, reactive ion beams or high-energy electron beams are generally adopted for processing, and the methods can accurately process high-precision micro-nano scale holes on the hard and brittle materials, but the methods have extremely high cost, complex operation and long processing time. In the reactive ion beam processing, for example, a through hole with a diameter of 30 μm is processed on a glass plate with a thickness of 150 μm for at least 10 hours, the market price of the reactive ion beam processing is 1000 yuan/hour, and an additional mask plate needs to be customized. Therefore, a method with low cost, simple operation and high processing efficiency is urgently needed for processing the through hole with the micro-nano scale on the hard and brittle material.
Disclosure of Invention
The invention aims to solve the problems of high cost and low efficiency of processing a micro-nano scale through hole on a hard and brittle material, and provides a method for processing the micro-nano scale through hole on a transparent hard and brittle material by femtosecond laser. The method comprises the steps of firstly forming a 4f beam shrinking system through a 150mm plano-convex lens and a 20 Xmicroscope objective (NA is 0.45), shrinking a Bessel beam formed through a 2-degree conical lens and focusing the Bessel beam on the surface of a sample, quantitatively adjusting the diameter of the Bessel beam and the movement of a six-freedom-degree precision displacement platform according to the target size range requirement of a micro-nano through hole to process a modified hole array, then putting the sample into a potassium hydroxide (KOH) solution to etch for a certain time, quantitatively removing the residual thickness of the sample by using a polishing machine, finally reversely putting the sample under an optical microscope or a scanning electron microscope to observe, and selecting the micro-nano through hole with the outlet size meeting the requirement range. The method adjusts the length of the modified hole by quantitatively controlling the incident light spot diameter of the Bessel beam, removes redundant materials by combining wet etching and quantitative polishing, flexibly adjusts the size of an outlet, has good adjustability, low cost and high processing efficiency, and can be applied to the fields of cell screening, DNA molecular sequencing and the like.
The purpose of the invention is realized by the following technical scheme:
the method for processing the micro-nano scale through hole on the transparent hard and brittle material by the femtosecond laser comprises the following specific steps:
the method comprises the following steps: designing the beam-shrinking magnification of the Bessel beam according to the target size range of the micro-nano through hole and the thickness of a sample to be processed, wherein the beam-shrinking system is used for adjusting the length of the beam and improving the energy density;
step two: the method comprises the following steps of respectively controlling the number of pulses and pulse energy irradiated on a glass sample by utilizing a mechanical switch and an attenuation sheet, and controlling a six-degree-of-freedom precision displacement platform to run a processing program by combining a computer control system to obtain a modified micron-scale blind hole array, wherein the tail end of each blind hole is provided with an inverted cone-shaped structure, and in the process, the material structure irradiated in the inner area of the sample by femtosecond laser is converted into a silicon-oxygen three-membered ring or a silicon-oxygen four-membered ring;
step three: the sample is put into KOH solution and ultrasonic oscillation is introduced for etching, and a silicon-oxygen three-membered ring or silicon-oxygen four-membered ring structure is more easily corroded by the KOH solution than a silicon-oxygen six-membered ring structure, so that a microchannel can be preferentially generated in a region processed by femtosecond laser, and an unmodified region is almost unchanged;
step four: because the tail end of the blind hole is conical, the larger the grinding and polishing removal thickness is, the larger the diameter of the outlet of the obtained micro-nano through hole is, and therefore, the residual thickness is removed quantitatively by using a grinding and polishing machine according to the designed size and dimension of the blind hole;
step five: and (4) placing the polished sample under an optical/scanning electron microscope, searching micro-nano through holes with the sizes of outlets in the array conforming to the target range, and marking the micro-nano through holes.
A device for processing micro-nano scale through holes on a transparent hard and brittle material based on space shaping femtosecond laser comprises a femtosecond laser system, an attenuation sheet, a mechanical switch, a conical lens, a plano-convex lens, a beam splitter, a white light source, a Charge Coupled Device (CCD), a dichroic mirror, a microscope objective, a six-degree-of-freedom precision displacement platform and a computer control system;
connection relation: the femtosecond laser system, the attenuation sheet, the mechanical switch, the conical lens, the plano-convex lens, the beam splitter, the white light source, the CCD, the dichroic mirror and the microscope objective are coaxially arranged, and a processing sample is arranged at the center of the six-degree-of-freedom precision displacement platform;
light path: after the femtosecond laser system generates Gaussian femtosecond laser, the laser energy is adjusted through an attenuation sheet, and the number of pulses irradiated to the surface of a sample is adjusted by controlling a mechanical switch through a computer control system; the adjusted laser beam forms a Bessel beam through a cone lens, and then is condensed and focused on the surface of a sample positioned at the center of a six-degree-of-freedom precision displacement platform through a beam shrinking system (a plano-convex lens and a microscope objective lens), wherein a dichroic mirror changes the direction of the beam so that the beam is vertically incident into the microscope objective lens; in the process, white light generated by the white light source passes through the beam splitter, the dichroic mirror and the microscope objective and then irradiates a processing area of the sample, then the white light returns to the beam splitter in the original path, and the beam splitter changes the propagation direction of reflected light and then enters the CCD, so that the real-time monitoring of the processing process is realized.
Advantageous effects
1. According to the method for processing the micro-nano through holes on the transparent hard and brittle materials by adopting the space-shaped femtosecond laser, the micro-nano through holes can be prepared on the transparent hard and brittle materials such as quartz glass, borosilicate glass, microcrystalline glass and Corning glass, and the application range is wide.
2. The femtosecond laser forms extremely high power density after being focused, so that the transparent material generates nonlinear absorption of energy only at the position of a focus, and the rapid coupling of the energy of an electron-lattice system greatly reduces a processing heat affected zone, can effectively inhibit the influence and thermal damage of various effects such as a melting zone, shock waves and the like on surrounding materials, and ensures good processing appearance. In addition, the average cost of processing a single hole by using the femtosecond laser is far lower than that of the existing method.
3. The method can process the N x N array micro-nano through holes at one time, so that the average single-hole processing time is greatly shortened compared with the existing method.
4. The method can continuously adjust the diffraction-free area of the Bessel beam according to the size range of the micro-nano through hole, and quantitatively adjust the outlet size of the micro-nano through hole within a certain range.
5. The method forms uniform modified zones in the femtosecond laser processing process, and assists ultrasonic oscillation in wet etching, so that the hole wall of the micro-nano scale through hole is smooth, and high-quality processing of the micro-nano scale through hole is realized.
Drawings
FIG. 1 is a schematic diagram for constructing a light path of the method for processing the micro-nano scale through hole on the transparent hard and brittle material by using the space shaping femtosecond laser.
FIG. 2 is a schematic diagram of a processing process of the method for processing the micro-nano scale through hole on the transparent hard and brittle material by the space shaping femtosecond laser.
FIG. 3 is a schematic diagram of micro-nano-scale through holes with outlet sizes meeting a target range, which are selected after the method is used for processing on a transparent hard and brittle material.
Fig. 4 is a scanning electron microscope image of an example of a through hole with an exit size of 325nm processed on a transparent hard and brittle material by the method of the present invention, and fig. 4(a) is a through hole with an exit size of 428 nm.
The system comprises a femtosecond laser system 1, an attenuation sheet 2, a mechanical switch 3, a cone lens 4, a plano-convex lens 5, a beam splitter 6, a white light source 7, a CCD 8, a dichroic mirror 9, a microscope objective 10, a sample 11, a precision displacement platform 12-six degrees of freedom 13 and a computer control system.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1
The method for processing the micro-nano scale through hole on the transparent hard and brittle material by the space shaping femtosecond laser comprises the following steps:
(1) as shown in figure 1, the femtosecond laser system 1 generates Gaussian laser with the wavelength of 800nm, the pulse width of 150fs and the repetition frequency of 1kHz, the energy of the laser is changed through the attenuation sheet 2, and the on-off of the mechanical switch 3 is controlled through the computer system 11. The Gaussian laser beam forms a Bessel beam through the conical lens 4, the Bessel beam enters the plano-convex lens 5 with the focal length of 150mm, the beam direction is changed through the dichroic mirror 9, and the beam vertically enters the microscope objective lens 10(20 x, NA is 0.45), wherein the combination of the plano-convex lens 5 and the microscope objective lens 10 forms a beam contraction system, and the energy density of the beam is improved; the beam-condensed and focused bessel beam is irradiated on the sample 11. In the process, white light emitted by the white light source 7 passes through the beam splitter 6, the dichroic mirror 9 and the microscope objective 10 to irradiate on a processing area of the sample 11 and returns to the beam splitter 6 along the original path, and the beam splitter 6 changes the propagation direction of the returned white light to the CCD 8 to observe the processing condition of the sample in real time.
(2) A corning glass sample 11 with the thickness of 200 mu m is fixed on a six-degree-of-freedom precision displacement platform 12, the laser power is adjusted to 10mW by using an attenuation sheet 2, and the number of deposited pulses of each modified hole is ensured to be 100 by using a mechanical switch. The incident light spot diameter can be adjusted, the length of the non-diffraction region is in direct proportion to the incident light spot diameter, in the embodiment, the incident light spot diameter is set to be 5mm, the cone base angle of the cone lens 4 is 2 degrees, the length Z of the non-diffraction region after passing through the 4f beam-shrinking system is calculated to be 162.9 μm, the upper surface of the sample 11 is arranged at the midpoint position of the non-diffraction region by the movable translation stage 12, the position is taken as a starting position, and the length of the non-diffraction region in the sample is 81.45 μm at the moment. Controlling the six-degree-of-freedom precision displacement platform 12 to move according to a set program through a computer control system 13, as shown in fig. 2, setting the program to machine a total of 100 modified holes (3 are used for replacing in the figure) in the positive direction of X, wherein delta X is 100 mu m; ② the movement in Y direction is 100 μm, at the same time the movement in Z direction is 0.1 μm; remachining 100 modified holes (3 in the figure) in the negative direction of X, wherein delta X is 100 mu m; and Y is 100 μm in the Y direction, and Z is 0.5 μm in the Z direction. Repeating the first step and the second step and the third step for 50 times to generate the modified wells with 100 multiplied by 100, wherein the modified wells have 100 different depths and the distance from the bottom of the sample ranges from 68.55 mu m to 118.55 mu m. The processing time for a single modified hole is only 0.1 second, and the processing time for 100 × 100 modified holes is less than 20 minutes.
(3) As shown in FIG. 2, the sample obtained in step (2) was removed, washed, and then etched in 35.8% KOH solution for 6 minutes (KOH etch modified region speed was about 800 μm/s). Due to the fact that the depth-diameter ratio of the modified hole is high, the solution is not prone to entering the interior of the modified hole in a standing state, and therefore ultrasonic vibration is introduced to enable the solution to better enter a modified area. The modified region of the siloxy three-or four-membered ring is more sensitive to KOH solution than the unmodified region of the siloxy six-membered ring, the ratio of etch rates of the former to the latter in 35.8% KOH solution being 200: 1, so that the volume of material removed in the unmodified region is negligible compared to the modified region in a short time. Because the modified area generated by the femtosecond laser is very uniform and ultrasonic oscillation is introduced, the side wall of the etched blind hole is very uniform. In addition, the bottom of the blind hole is conical, and the conical angle is about 12.8 degrees.
(4) And (4) polishing and removing the bottom of the sample obtained in the step (3) by using a polishing machine, wherein the removal height is calculated to be 69.89-70.56 microns, for example, through holes with the outlet size ranging from 300nm to 450nm are obtained. And (3) reversely placing the obtained sample under an optical/scanning electron microscope after the grinding and polishing are removed, and observing and selecting through holes which accord with the target size of 300 nm-450 nm in an outlet array and marking the through holes as shown in figure 3.
(5) As shown in FIG. 4, through holes with outlet sizes of 325nm [ FIG. 4(a) ] and 428nm [ FIG. 4(b) ] are found in the array, and whether to cut and take out can be determined according to actual needs. If the thickness which is carelessly removed during grinding and polishing is larger than the calculated thickness, the height can be recalculated and removed by virtue of the same taper angle at the bottom of the blind hole array and 100 different heights, and the grinding and polishing are continuously performed.
Finally, the method for processing the micro-nano-scale through hole on the transparent hard and brittle material based on the space shaping femtosecond laser is low in cost and high in efficiency, and the micro-nano-scale through hole suitable for cell screening and DNA molecule sequencing is prepared.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. The method for processing the micro-nano scale through hole on the transparent hard and brittle material by the femtosecond laser is characterized in that: focusing the shrunk Bessel beam on the surface of a sample, quantitatively adjusting the diameter of the Bessel beam according to the target size range requirement of the micro-nano through hole, further adjusting the length of a modified hole, and moving the sample to perform modified hole array processing; the modified hole is a blind hole, and the tail end of the blind hole is provided with an inverted cone-shaped structure; after a sample is put into a corrosive solution for etching for a certain time, the rest thickness is removed quantitatively by a grinding and polishing machine according to the size and the dimension of a designed blind hole, finally the sample is reversely placed under an optical microscope or a scanning electron microscope for observation, and a micro-nano through hole with the outlet size meeting the requirement is selected;
the etching solution comprises a KOH solution.
2. The method of claim 1, wherein: the beam shrinking method comprises the following steps: and determining the beam-shrinking magnification of the Bessel beam according to the outlet target size range of the micro-nano through hole and the thickness of the sample to be processed, wherein the beam-shrinking system is used for adjusting the length of the beam and improving the energy density.
3. The method of claim 1, wherein: the method for processing the modified hole array comprises the following steps: the method comprises the steps of utilizing a mechanical switch and an attenuation sheet to respectively control the number of pulses and pulse energy irradiated on a glass sample, and combining a computer control system to control a six-degree-of-freedom precision displacement platform to operate a machining program to obtain a modified micron-scale blind hole array, wherein the tail end of each blind hole is provided with an inverted cone-shaped structure, and in the process, the material structure irradiated in the inner area of the sample by femtosecond laser is converted into a silicon-oxygen three-membered ring or a silicon-oxygen four-membered ring.
4. The method of claim 1, wherein: the method for quantitatively removing the residual sample thickness comprises the following steps: because the tail end of the blind hole is conical, the larger the grinding and polishing removal thickness is, the larger the diameter of the outlet of the obtained micro-nano through hole is, and therefore, the residual thickness is removed quantitatively by using a grinding and polishing machine according to the designed size and dimension of the blind hole.
5. The method of any of claims 1 to 4, wherein: the required device comprises a femtosecond laser system, an attenuation sheet, a mechanical switch, a conical lens, a plano-convex lens, a beam splitter, a white light source, a charge coupling device, a dichroic mirror, a microscope objective, a six-degree-of-freedom precision displacement platform and a computer control system;
after the femtosecond laser system generates Gaussian femtosecond laser, the laser energy is adjusted through an attenuation sheet, and the number of pulses irradiated to the surface of a sample is adjusted by controlling a mechanical switch through a computer control system; the adjusted laser beam forms a Bessel beam through a cone lens, and then the beam is condensed and focused on the surface of a sample positioned at the center of a six-degree-of-freedom precision displacement platform through a beam shrinking system, wherein a dichroic mirror changes the direction of the beam so that the beam is vertically incident into a microscope objective; in the process, white light generated by the white light source passes through the beam splitter, the dichroic mirror and the microscope objective and then irradiates a processing area of a sample, then the white light returns to the beam splitter in the original path, and the beam splitter changes the propagation direction of reflected light and then irradiates the reflected light into the charge coupled device, so that the real-time monitoring of the processing process is realized.
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| CN113909710A (en) * | 2021-10-28 | 2022-01-11 | 帝尔激光科技(无锡)有限公司 | Method and equipment for processing micropores |
| CN115138997B (en) * | 2022-09-07 | 2022-12-06 | 武汉引领光学技术有限公司 | Multipoint Bessel beam glass punching device and method |
| CN117548861A (en) * | 2024-01-10 | 2024-02-13 | 深圳市大族数控科技股份有限公司 | Method and system for processing slotted hole in light-transmitting material |
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