CN103706955A - Method for preparing high depth-diameter-ratio three-dimensional micro-channel through electronic dynamic control - Google Patents
Method for preparing high depth-diameter-ratio three-dimensional micro-channel through electronic dynamic control Download PDFInfo
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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
- B23K26/40—Removing material taking account of the properties of the material involved
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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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
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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
- B23K26/361—Removing material for deburring or mechanical trimming
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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
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Abstract
The invention relates to a method for preparing a high depth-diameter-ratio three-dimensional micro-channel through electronic dynamic control, and belongs to the technical field of femtosecond laser applying. The time domain shaping is carried out on a femtosecond laser, the partial instant electronic dynamic condition ( especially the freedom electron density distribution), of a modified area is regulated and controlled, the appearance of a periodicity nanometer structure of the modified area is affected, the high depth-diameter-ratio three-dimensional micro-channel irrelative to polarization can be achieved, and compared with a traditional femtosecond laser machining method, the method has the advantage that the depth-diameter-ratio can be multiply increased during the three-dimensional micro-channel machining.
Description
Technical field
The present invention relates to a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation, belong to femtosecond laser applied technical field.
Background technology
High aspect ratio three dimension microchannels are the key structures in microfluidic device, because it can control indivisible liquid with very high precision, can minimization chemical-biological analytical system size also further improve its integrated level, have attracted numerous concerns.Take quartz glass as main silicon-dioxide-substrate transparent material is due to its good optics, chemistry and thermal property, be to build the ideal substrate of many microfluid systems.
At present, in microfluid system, the manufacture of microchannel mainly depends on the method for photoetching, and the inherent limitations of the method is to carry out surperficial two dimensional surface manufacture.So when manufacturing three-dimensional microfluidic systems, the layering of having to manufactures that laggard windrow is folded, bonding and encapsulation, needs a plurality of masks, has increased cost and the complexity manufactured, and the bonding agent using during bonding easily leaks in microchannel, affects its practical application.Laser is fabricated to high efficiency high-quality microchannel processing possibility is provided.The development of ultrafast laser, particularly femtosecond laser more becomes the effective tool of preparing micro-structural on transparent material.Due to the ultrashort pulsewidth of femtosecond laser and the peak power density of superelevation, can reduce greatly heat affected area, improve machining accuracy and quality.Femtosecond laser modification Assisted Chemical Etching Process is a technical way that utilizes femtosecond laser processing microchannel.The method of femtosecond laser modification Assisted Chemical Etching Process is mainly divided into two steps: 1) use the tight femto-second laser pulse focusing on to scan default three-dimensional structure shape at material internal, make scanning area generation chemical modification; 2) use etching agent solution to carry out etching to there is the region of modification, obtain the MCA of hollow.Difference due to laser parameter (pulsewidth, energy, polarization etc.), focused condition (processing numerical aperture of objective, the depth of focus etc.) and properties of materials, will produce three kinds of different modification results: the 1) variation of Refractive Index of Material; 2) modification area forms the periodicity nanometer grating structure vertical with laser polarization direction; 3) material microburst forms the destructive modification of cavity.Thereby discovery the second modifications such as Hantovsky can obtain maximum Etch selectivity and realize higher aspect ratio, yet there is correlation in the nanostructured and the polarization that due to this modification area, form, has certain difficulty when machining 3 D microchannel.
Summary of the invention
The object of the invention is to machining 3 D microchannel, to cause difficult problem in order to solve the correlation of modification area nanostructured and polarization, a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation is provided.By femtosecond laser is carried out to time domain shaping, regulate and control the Local Instantaneous electronic Dynamic (being mainly free electron density distributes) of modification area, thereby affect the pattern of its periodic nano-structure.
The object of the invention is to realize by following technology:
A method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation, concrete steps are as follows:
Step 1: produce femto-second laser pulse, pulsewidth is greater than 30 femtoseconds and is less than 100 femtoseconds.
Step 2: the femto-second laser pulse energy that set-up procedure one obtains, makes energy between the modification energy threshold and ablation energy threshold of institute's processed sample.
Step 3: the femto-second laser pulse that step 2 is obtained is modulated to the laser pulse sequence at femtosecond interval, every group of laser pulse sequence comprises a plurality of femtosecond pulses, adjacent femto-second laser pulse be spaced apart femtosecond, be greater than 500 femtoseconds and be less than 3000 femtoseconds.
Described laser pulse interval can guarantee that free electron Energy Coupling efficiency that in set of pulses sequence, postorder pulse and preorder pulse produce is greater than the Energy Coupling efficiency of single femto-second laser pulse and material, and can regulate and control the coupled field of electronic Dynamic and laser field, obtain latticed periodic nano-structure, eliminate the impact of polarization on modification area etching performance.
Step 4: the laser pulse sequence that step 3 is obtained focuses on by processing object lens, processed sample is positioned on the sextuple mobile displacement platform of energy, controls displacement platform and drives processed sample to move, and utilizes laser spot according to design drawing requirement, sample to be processed; Sample interior laser spot track while scan the material of process form modification.
The focal length of processing object lens is greater than the depth capacity that laser spot processing reaches.
Step 5: the sample of the modification of step 4 gained is placed in to chemical solution and carries out chemical etching.If need, accelerate etching energy and introduce ultrasonic vibration.
Described processed sample material is the transparent glass material of silica (SiO2) base.
Described chemical solution is for and producing the solution of Etch selectivity (modification area etch rate is greater than unmodified region) with silicon dioxde reaction.Its concentration requirement is between 5% to 20%.
Beneficial effect:
1, a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation of the present invention, can realize the high aspect ratio microchannel processing with polarization decorrelation.
2, a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation of the present invention, compares with traditional femtosecond laser processing method, and when machining 3 D microchannel, its aspect ratio can improve several times.
Accompanying drawing explanation
Fig. 1 is in specific embodiment, femto-second laser pulse serial processing index path:
Fig. 2 is that the femtosecond laser focusing in specific embodiment is processed partial enlarged drawing in material internal modification:
Wherein, 1-fs-laser system, 2-the first half-wave plate, 3-polarizer, 4-pulse shaper, 5-the second half-wave plate, 6-light-operated switch, 7-speculum, 8-dichroscope, 9-focusing objective len, 10-sample, the sextuple precision displacement platform of 11-, 12-lighting source, 13-imaging CCD.
The specific embodiment
Below in conjunction with drawings and Examples, the present invention will be further described.
The device of realizing the inventive method in this specific embodiment comprises: fs-laser system, the first half-wave plate, the second half-wave plate, polarizer, electric-controlled switch, pulse shaper, speculum, focusing objective len, dichroscope, sextuple precision displacement platform.
Its annexation is for as shown in Figure 1.Fs-laser system 1, the first half-wave plate 2, polarizer 3, pulse shaper 4, the second half-wave plate 5, light-operated switch 6 be parallel, coaxially placement in turn, and speculum 7 is positioned at light-operated switch 6 opposite sides, placement at 45 °.Being centered close on the optical axis being reflected after mirror 7 reflections of dichroscope 8, placement at 45 °.Optical axis after reflection is successively by dichroscope 8, focusing objective len 9, sample 10, sextuple precision displacement platform 11, lighting source 12 center.Imaging CCD13 receives the reverberation of dichroscope 8.Fs-laser system 1 produces femto-second laser pulse, utilize the first half-wave plate 2 and the combination of polarizer 3 to adjust after energy, enter pulse shaper 4 and be modulated to laser pulse sequence, laser pulse sequence regulates polarization through half-wave plate 5, thereafter light-operated switch 6 is used for controlling laser break-make, and then laser pulse sequence is reflected mirror 7 and is reflected into focusing objective len 9 focusing that are arranged in sextuple precision displacement platform 11 tops.Sample 10 is fixed on sextuple precision displacement platform 11, and by the lighting source 12 generation illumination light of platform 11 belows, illumination light enters imaging CCD13 imaging after sample 10, focusing objective len 9, dichroscope 8, to monitor in real time process.
What fs-laser system 1 adopted is the laser instrument that U.S.'s spectrum physics (SpectraPhysics) company produces, optical maser wavelength 800nm, and pulse width 50 femtoseconds, repetition rate 1KHz is adjustable, pulse ceiling capacity 3mJ, light distribution is Gaussian, linear polarization.
A kind of method of preparing high aspect ratio three dimension microchannels by femto-second laser pulse sequence that the present invention proposes, as shown in Figure 1, concrete procedure of processing is as follows for processing light path:
Step 1: utilize fs-laser system 1 to produce femtosecond pulse, utilize the combination of half-wave plate 2 and polarizer 3 that single pulse energy is adjusted into 0.5 μ J, by pulse shaper 4, femtosecond laser is modulated to pulse train, in this sequence, comprise two subpulses, pulse spacing is 1000 femtoseconds, by the polarization state of polarizer 5 regulating impulse sequence laser, by the break-make of light-operated switch control 6 laser processed;
Step 2: the resulting pulse train laser of step 1 is reflexed in 50 times of processing object lens 9 and focused on by speculum 7, by CCD13 and lighting source 12 imagings, vitreous silica sample 10 is fixed on sextuple precision displacement platform 11, the sextuple precision displacement platform 11 that computerizeds control moves, and laser spot is positioned on the upper surface of sample 10 of horizontal positioned;
Step 3: by the sextuple precision displacement platform 11 100 μ m that move up, make laser spot be positioned at the following 100 μ m of sample upper surface, as shown in Figure 2, mobile platform 11 makes laser spot along directions X horizontal movement, form the material modification of sample interior, regulate polarizer 5 can make laser polarization direction, electric field intensity direction E and X in the same way or with Y in the same way.
Step 4: the HF solution that the sample of the modification of step 3 gained is placed in to 10% concentration carries out sonochemistry etching 1 hour, can etch the MCA with certain aspect ratio.
When not using pulse shaper 4 or pulse daley being set to zero, in the immovable situation of other experimental procedures, be to process with traditional femtosecond laser processing method.Use conventional laser, when pulse energy is 0.5 μ J, because modification area can form the periodicity nanometer grating structure vertical with polarization direction, when θ shown in Fig. 2 is 0 °, E and X are in the same way time, and the microchannel degree of depth obtaining is 75 μ m, and shown in θ be 90 °, be E and Y in the same way time, the microchannel degree of depth obtaining is 505 μ m, and the difference of bringing due to the impact of polarization is 430 μ m.When the 1000fs that uses this method to propose postpones dipulse serial processing, by the regulation and control to modification area Local Instantaneous electronic Dynamic (free electron density distribution), when θ is 0 °, be E and X in the same way time, the microchannel degree of depth obtaining is 485 μ m, and shown in θ be 90 °, be that E and Y are in the same way time, the microchannel degree of depth obtaining is 525 μ m, and the difference of bringing due to the impact of polarization is reduced into only 40 μ m, and the diameter of above-mentioned microchannel is approximately 12 μ m all.Consider the error of experiment, can think that the high aspect ratio microchannel that can realize the correlation of depolarizing when using pulse train processes.
What fs-laser system 1 adopted is the laser instrument that U.S.'s spectrum physics (SpectraPhysics) company produces, optical maser wavelength 800nm, and pulse width 50 femtoseconds, repetition rate 1KHz is adjustable, pulse ceiling capacity 3mJ, light distribution is Gaussian, linear polarization.
A kind of method of preparing high aspect ratio three dimension microchannels by femto-second laser pulse sequence that the present invention proposes, as shown in Figure 1, concrete procedure of processing is as follows for processing light path:
Step 1: utilize fs-laser system 1 to produce femtosecond pulse, utilize the combination of half-wave plate 2 and polarizer 3 that single pulse energy is adjusted into 0.5 μ J, by pulse shaper 4, femtosecond laser is modulated to pulse train, in this sequence, comprise two subpulses, pulse spacing is 1000 femtoseconds, by the polarization state of polarizer 5 regulating impulse sequence laser, by the break-make of light-operated switch control 6 laser processed;
Step 2: the resulting pulse train laser of step 1 is reflexed in 50 times of processing object lens 9 and focused on by speculum 7, by CCD13 and lighting source 12 imagings, vitreous silica sample 10 is fixed on sextuple precision displacement platform 11, the sextuple precision displacement platform 11 that computerizeds control moves, and laser spot is positioned on the upper surface of sample 10 of horizontal positioned;
Step 3: by the sextuple precision displacement platform 11 100 μ m that move up, make laser spot be positioned at the following 100 μ m of sample upper surface, mobile platform 11 make laser spot the track of sample interior scanning square-wave form or circular arc from but material generation modification;
Step 4: the HF solution that the sample of the modification of step 3 gained is placed in to 10% concentration carries out sonochemistry etching 1 hour, can etch the MCA with certain aspect ratio.
When not using pulse shaper 4 or pulse daley being set to zero, in the immovable situation of other experimental procedures, be to process with traditional femtosecond laser processing method.Use conventional laser, when pulse energy is 0.5 μ J, because modification area can form the periodicity nanometer grating structure vertical with polarization direction, when microchannel direction is parallel with polarization direction, etch rate can sharply reduce even to stop.When the 1000fs that uses this method to propose postpones dipulse serial processing, thereby regulate and control its Etch selectivity by rational regulation and control modification area Local Instantaneous electronic Dynamic, its length of square waveform microchannel of gained is 4-5 times while using conventional laser, its length of circular arc microchannel of gained is 7 times while using conventional laser, has represented the advantage of this method when machining 3 D microchannel.
Claims (4)
1. a method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation, is characterized in that: concrete steps are as follows:
Step 1: produce femto-second laser pulse, pulsewidth is greater than 30 femtoseconds and is less than 100 femtoseconds;
Step 2: the femto-second laser pulse energy that set-up procedure one obtains, makes energy between the modification energy threshold and ablation energy threshold of institute's processed sample;
Step 3: the femto-second laser pulse that step 2 is obtained is modulated to the laser pulse sequence at femtosecond interval, every group of laser pulse sequence comprises a plurality of femtosecond pulses, adjacent femto-second laser pulse be spaced apart femtosecond;
Described laser pulse interval can guarantee that free electron Energy Coupling efficiency that in set of pulses sequence, postorder pulse and preorder pulse produce is greater than the Energy Coupling efficiency of single femto-second laser pulse and material, and can regulate and control the coupled field of electronic Dynamic and laser field, obtain latticed periodic nano-structure;
Step 4: the laser pulse sequence that step 3 is obtained focuses on by processing object lens, processed sample is positioned on the sextuple mobile displacement platform of energy, controls displacement platform and drives processed sample to move, and utilizes laser spot according to design drawing requirement, sample to be processed; Sample interior laser spot track while scan the material of process form modification;
The focal length of processing object lens is greater than the depth capacity that laser spot processing reaches;
Step 5: the sample of the modification of step 4 gained is placed in to chemical solution and carries out chemical etching;
The transparent glass material that described processed sample material is silicon-dioxide-substrate;
Described chemical solution makes modification area etch rate be greater than unmodified region solution for and producing Etch selectivity with silicon dioxde reaction.
2. a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation according to claim 1, is characterized in that: the interval of described adjacent femto-second laser pulse is greater than 500 femtoseconds and is less than 3000 femtoseconds.
3. a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation according to claim 1, is characterized in that: introduce Under Ultrasonic Vibration kinetic energy and accelerate chemical etching.
4. a kind of method of utilizing high aspect ratio three dimension microchannels of electronic Dynamic regulation and control preparation according to claim 1, is characterized in that: chemical solution concentration is between 5% to 20%.
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| CN103909352A (en) * | 2014-04-25 | 2014-07-09 | 北京理工大学 | Femtosecond laser processing method for achieving electronic state regulation and control based on local ion implantation |
| CN104591549A (en) * | 2014-12-29 | 2015-05-06 | 北京理工大学 | Method for processing micro array on glass surface via femtosecond laser pulse sequence |
| CN104625438A (en) * | 2014-12-29 | 2015-05-20 | 中自高科（苏州）光电有限公司 | Method for manufacturing micro channel by combining laser polarization selective ablation with acid etching |
| CN106041313A (en) * | 2016-06-22 | 2016-10-26 | 中南大学 | Uniform modification processing method of transparent medium microstructures |
| CN106216833A (en) * | 2016-08-10 | 2016-12-14 | 北京理工大学 | Method based on dynamic control laser machine semiconductor twin-stage surface texture |
| CN107088703A (en) * | 2017-06-12 | 2017-08-25 | 北京理工大学 | Oval lenticule processing method based on dynamic control and chemical auxiliary etch |
| CN107283047A (en) * | 2017-08-07 | 2017-10-24 | 南方科技大学 | One kind prepares non-crystaline amorphous metal device, method and application using pulse laser |
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| CN108637501A (en) * | 2018-04-13 | 2018-10-12 | 杭州电子科技大学 | The molding control method of silicon substrate internal microstructure based on Laser Ultrasonic Technique |
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