CN106735947A - A kind of method of efficiently controllable processing bulk silicon micro-nano structure - Google Patents
A kind of method of efficiently controllable processing bulk silicon micro-nano structure Download PDFInfo
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- 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
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
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- 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
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- 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
- B23K26/0626—Energy control of the laser beam
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- 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
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/50—Working by transmitting the laser beam through or within the workpiece
- B23K26/53—Working by transmitting the laser beam through or within the workpiece for modifying or reforming the material inside the workpiece, e.g. for producing break initiation cracks
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
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- B23K2101/00—Articles made by soldering, welding or cutting
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Abstract
The present invention relates to a kind of method of efficiently controllable processing bulk silicon micro-nano structure, belong to femtosecond laser applied technical field.Method of the present invention based on chemical etching auxiliary femtosecond laser processing and flight time punching, effectively using femtosecond laser is ultrafast, superpower, ultraprecise processing characteristic, efficient controllable processing large area micro-nano structure within a short period of time；Specifically cause that silicon face forms partial modification area under the effect of single laser pulse, the chemism in laser irradiation region domain drastically declines, so as to play a part of mask in subsequent chemistry etching process, and then realize the processing without mask high-effect high-quality silicon micro-nano structure.Contrast prior art, present invention omits in rapidoprint plated surface mask layer step, processing efficiency is improve while reduces cost, while also allowing for operating and controlling, realizes that the bulk silicon surface micro-nano structure under different-shape and size is accurate, controllability processing；Process velocity is limited only in laser pulse repetition frequency.
Description
Technical field
It is more particularly to a kind of to combine chemistry the present invention relates to a kind of method of efficiently controllable processing bulk silicon micro-nano structure
The method of the efficient controllable processing bulk silicon micro-nano structure of etching auxiliary femtosecond laser, belongs to femtosecond laser applied technical field.
Background technology
Silicon crystal material is semi-conducting material more important at present, has high index of refraction and energy active set mainly due to it
Into among the microelectronic component to complexity.Controllable appearance and arrangement silicon face micro-nano structure microelectronics, photon, photoelectricity volt,
There is extremely important application in the fields such as microfluid, wetting characteristics, solar cell and sensor.The silicon face of different-shape is micro-
Micro-nano structure can be obtained by different processing methods, such as photoetching technique, nanometer embossing and dry etching technology etc..
In recent years, femtosecond laser process technology is because with high accuracy, low re cast layer, contactless, heat affected area is small and processes
Flexibly the advantages of, it is considered to be the maximally effective machining tool of Precision Machining micro-nano structure on solid material.Micropore, microflute,
The micro-nano structure of the forms such as microprotrusion, micro-nano compound structure and nano particle can be processed by femtosecond laser direct writing technology
Arrive.In addition, the processing to better control over micro-nano structure form, introduces chemical quarter on the basis of femtosecond laser process technology
Erosion secondary process.Traditional chemistry auxiliary femtosecond laser process technology, need in advance on processed sample plated surface silica or
The mask layer of silicon nitride, mask layer, the silicon base for then exposing quilt in etching solution are locally removed through Gold Films Irradiated by Femtosecond Laser
Etching, forms the micro-nano structure of different-shape.But above-mentioned processing method needs additional processing mask layer before processing, and this not only increases
Cost is added and so that processing efficiency has been substantially reduced.
The content of the invention
Bulk silicon nanometer lattice row processing efficiency the invention aims to solve existing high-quality, high homogeneity
Relatively low, relatively costly problem, it is proposed that one kind combines chemical etching auxiliary femtosecond laser, and efficiently controllable processing bulk silicon is micro-
The method of micro-nano structure.
Principle of the invention is directly irradiated by femtosecond laser, regulates and controls the electron density of laser irradiation region domain transient state, is changed
Become the local chemism of material, and then regulate and control the etch rate of modified zone during chemical etching, and combine femtosecond laser and " fly
Row time punch method " (Journal of Laser Applications, 4 (2), 15-24,1992), realizes bulk silicon micro-nano
The efficient controllable processing of structure.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method of the efficient controllable processing bulk silicon micro-nano structure of combination chemical etching auxiliary femtosecond laser, specific step
It is rapid as follows：
Step one, femtosecond laser beam is focused on using microcobjective；
Step 2, adjusts laser energy：Using half-wave plate-polarizer combination regulation laser energy so that laser pulse energy
Amount is less than the ablation threshold on rapidoprint surface, and pulsed laser energy can be continuously adjusted；
Step 3, mobile platform is fixed on by rapidoprint, and regulation mobile platform makes femto-second laser pulse focus on processing
Material surface；
Step 4, utilizes " flight time punch method ", realizes the large area highly-efficient processing under the conditions of femtosecond laser pulse；
Step 5, the chemical solution that the rapidoprint after femtosecond laser processing in step 4 is placed under the certain concentration of constant temperature
In liquid, after etched time t, obtain that surface is smooth and uniform high quality silicon micro-nano structure.
Preferably, the different-shape and chi of use requirement can be met by controlling laser flux, etch period
The very little micro-nano structure, and the spacing of adjacent structure can be controlled by controlling pulse laser repetition rate, sweep speed.
The monocrystalline silicon preferably, N-type that rapidoprint described in step 3 is 100 crystal orientation undopes.
Preferably, the etching solution is potassium hydroxide (KOH) solution, concentration is 25wt%, and thermostat temperature is 55 DEG C,
Etch period t is between 30s to 120s.
Beneficial effect
Existing silicon nano dots array process technology is contrasted, a kind of chemical etching that combines proposed by the present invention aids in femtosecond laser
The method of highly-efficient processing bulk silicon nano-dot matrix array structure has the characteristics that：
1st, the present invention irradiates to form partial modification area by femtosecond laser pulse, and this modification area can be directly as quarter
Mask during erosion, is eliminated in processed sample plated surface mask layer step, and processing efficiency is improve while reduces cost；
2nd, the rapidoprint after being processed to femtosecond laser is etched using chemical solution, is covered relative in processed sample plated surface
Film layer, is easy to operate and controls；
3rd, process velocity is limited only in laser pulse repetition frequency, if laser repetition rate is fast with the displacement of rapidoprint
The upper limit of degree is higher, and processing efficiency can be further improved in theory；
4th, by regulating and controlling femtosecond laser energy size, the bulk silicon surface micro-nano under different-shape and size can be realized
Precise structure, controllability processing, to adapt to the application demand under different occasions.
Brief description of the drawings
Fig. 1 combines chemical etching and aids in femtosecond laser highly-efficient processing bulk silicon nano-dot matrix array structure for the present invention is a kind of
Device structural representation.
Fig. 2 combines chemical etching and aids in femtosecond laser highly-efficient processing bulk silicon nano-dot matrix array structure for the present invention is a kind of
Method and step schematic diagram.
Reference：1- fs-laser systems, 2- half-wave plates, 3- polarization splitting prisms, the continuous attenuators of 4-, 5- reflections
Mirror, 6- mechanical shutters, 7- dichroscopes, 8- focus on microcobjective, 9- rapidoprints, 10- 6 DOFs precision displacement platform, 11- bis-
To Look mirror A, 12- planoconvex spotlight, 13-CCD imageing sensors, 14- imaging illumination light sources.
Specific embodiment
The preferred embodiment of the present invention is described further with reference to Figure of description and embodiment.
Realized in the present embodiment the inventive system comprises：Fs-laser system 1, half-wave plate 2, polarization splitting prism 3, company
Continuous attenuator 4, speculum 5, mechanical shutter 6, dichroscope 7, focusing microcobjective 8, sextuple precision displacement platform 10 and chemistry
The glass beaker vessel of water bath heating device and carrying etching solution needed for etching.
Its annexation is as depicted in figs. 1 and 2.Fs-laser system 1, half-wave plate 2, polarization splitting prism 3, continuous decay
Piece 4 is parallel successively, coaxial placement, and speculum 5 is coaxial with continuous attenuator 4 and mutual placement at 45 °；Mechanical shutter 6 and reflection
Mirror 5 is coaxial and mutually at 45 °, and dichroscope 7 is centrally located at the central shaft of mechanical shutter 6 and focuses on the central shaft of microcobjective 8
Focal position, and placement at 45 °；Laser beam axis pass sequentially through focusing microcobjective 8, rapidoprint 9 through the reflection of dichroscope 7
Center.For ease of operating personnel's monitor in real time process, it is added on said apparatus as lighting source and image sensing
Device, the two composition frontal imaging system carries out real time imagery to process；Lighting source is located at sextuple precision displacement platform
Top, the illumination light that it sends transmits dichroscope A11, dichroscope 7 successively, and line focus microcobjective 8 is radiated at sextuple essence
On rapidoprint 9 on close displacement platform 10, machined material 9 reflect after through focus on microcobjective 8, dichroscope 7 by two to
Focused on through planoconvex spotlight 12 after Look mirror A11 reflections and enter the formation real-time monitored image of ccd image sensor 13.
It is the ultra-short pulsed femtosecond laser of 800nm that femtosecond laser 1 produces centre wavelength, using half-wave plate 2 and polarization spectro
The combination of prism 3 can in a big way it is interior regulation and control laser pulse flux, then further can continuously be changed using continuous attenuator 4
Laser flux, changes the direction of laser beam by speculum 5, mechanical shutter 6 be used for controlling laser beam by whether,
So as to control laser beam to realize processing；Gaussian beam is focused using microcobjective 8 is focused on, realizes breaking through diffraction
The high-resolution processing of the limit；Rapidoprint 9 is fixed on sextuple precision displacement platform 10, by the imaging processed above light path
Lighting source 14 produces illumination white light, and illumination light reaches rapidoprint by dichroscope A11, dichroscope 7 and focusing objective len 8
Surface, the illuminating ray of the then reflection of machined material 9 is returned along original route, and ccd image is entered after being reflected by dichroscope A11
Sensor 13 is imaged, and monitor in real time can be carried out to rapidoprint surface in laser processing procedure.Gold Films Irradiated by Femtosecond Laser is processed
After the surface of material 9 forms large area modified Nano structural region, insert in the alkaline solution of constant temperature, such as potassium hydroxide (KOH),
NaOH (NaOH), tetramethyl aqua ammonia (TMAH) solution etc., carry out chemical etching such that it is able to obtain large area, height
The silicon micro-nano structure of quality.
Embodiment
Fs-laser system swashing using the production of U.S.'s spectrum physics (Spectra Physics) company in the present embodiment
Light device, laser center wavelength is 800nm, pulse width 35fs, and repetition rate 1KHz is adjustable, pulse ceiling capacity 3mJ, light intensity
It is distributed as Gaussian, linear polarization.
Rapidoprint 9 is the monocrystalline silicon of N-type non-impurity-doped crystal orientation 100, and its size is 10mm × 10mm × 1mm.Certainly, ability
Field technique personnel know, reality processing thing is not limited to monocrystalline silicon, its can be it is any other can by laser irradiate changeization
Learn the material of characteristic.
A kind of combination chemical etching proposed by the present invention aids in the side of femtosecond laser highly-efficient processing bulk silicon micro-nano structure
Respectively as depicted in figs. 1 and 2, specific procedure of processing is as follows for method, processing index path and experimental procedure schematic diagram：
Step one：Femtosecond pulse is produced using fs-laser system 1, half-wave plate 2 and polarization splitting prism 3 can be both used
Regulation single-pulse laser flux is in 0.14J/cm2, it is also possible to the continuous regulation of attenuator 4 laser flux reaches analog value.By control
The Push And Release of mechanical shutter processed 5 controls whether laser beam can be processed.
Step 2：Gaussian beam vertical incidence in step one is entered 20 × focusing microcobjective 8 (Olympus, NA=
0.45), the laser spot diameter after focusing is about 2.2 μm.
Step 3：The monocrystal silicon sample 9 of 100 crystal orientation is fixed on sextuple precision displacement platform 10, computer program is used
Control moving up and down for sextuple precision displacement platform 10 so that be processed the surface of sample 9 and be in femtosecond laser focussing plane.Borrow
Furtherance is as lighting source 14 and the composition frontal imaging system of imageing sensor 13, real-time monitored process.
Step 4：Utilize " flight time punch method ", regulation femtosecond laser repetition rate to 200Hz is compiled by computer
Journey programme-control 6 DOF precision displacement platform 10 is at the uniform velocity moved, and its translational speed is set as 2mm/s, is capable of achieving pulse processing big
Area nanometer lattice array, the spacing of adjacent nano point is 10 μm.By that analogy, sextuple precision displacement platform is controlled to enter rapidly automatically
Line period zigzag scanning is processed, and is capable of achieving the high efficiency processing in bulk silicon nano dot partial modification region.
Step 5：Concentration is inserted in water bath heating device for the KOH solution of 25wt% and is heated, when temperature reaches 55
DEG C when stop heat and cause temperature it is constant at 55 DEG C, the silicon sample after Gold Films Irradiated by Femtosecond Laser in step 4 is placed in etching solution
Middle constant temperature etches 60s, is then cleaned by ultrasonic 5min using acetone, alcohol, distilled water respectively, you can obtain high-quality, height homogeneous
The bulk silicon nano-dot matrix array structure of property.One skilled in the art will appreciate that etching solution KOH is based on processed sample monocrystalline silicon
Chemical characteristic and select, suitable etching solution can be selected according to the chemical characteristic of respective material for other materials.
The different-shape of use requirement and the micro-nano structure of size are met by controlling laser flux, etch period,
Such as class annular silicon column structure, flat-top shape silicon column structure and silicon nano dots structure, by controlling pulse laser repetition rate, scanning speed
The spacing of degree control adjacent structure.On the premise of sweep speed is sufficiently large, set pulse frequency is higher, and processing efficiency is higher.
In the present embodiment, when using 0.14J/cm2Pulse laser flux and chemical etching time 60s when, using single-pulse laser plus
The diameter of work gained silicon nano dots is about 313nm, is highly 200nm or so.It is 200Hz, accurate displacement in laser repetition rate
When the translational speed of platform 10 is 2mm/s, can be uniform on the monocrystal silicon sample 9 of 1cm × 1cm sizes using only about 85 minutes
100,200,1 high-quality nano-dot matrix array structures of nano dot are processed, the spacing of its adjacent nano point is 10 μm.Work as increase
During laser energy, 0.40J/cm is used2Pulse laser flux and chemical etching time 60s when, processed using single-pulse laser
The diameter of gained flat-top shape silicon column structure is about 1.20 μm, is highly 250nm or so.Further increase laser energy, when using
0.93J/cm2Pulse laser flux and chemical etching time 60s when, then class ring can be obtained under single-pulse laser processing conditions
Shape silicon column structure, its outer annular diameter is about 1.70 μm, and outer shroud is highly about 220nm, and annular diameters are about 1.37 μm, are highly about
230nm.Similarly, under the premise of adjacent structure is nonoverlapping, can be controlled according to regulation and control laser pulse repetition frequency and sweep speed
The spacing of adjacent micro-nano structure in large area array structure processed, for example, the use of repetition rate being 200Hz, sweep speed is 2mm/
S, its spacing is 10 μm；Repetition rate is constant, and when sweep speed is changed into 1mm/s, then the spacing of adjacent micro-nano structure is changed into 5 μm.
In order to process the micro-nano structure of different-shape and size, different etch periods can be selected, but etch period t should
In the range of 30s to 120s, because if etch period is too short, it is not able to form micro-nano structure on rapidoprint surface；Carve
Erosion overlong time, the mask effect of the modification area of chemism reduction is drastically reduced with the growth of etch period, gained
The surface of micro-nano structure is partially etched, and surface roughness is increased dramatically, and surface quality is reduced and height is also decreased.Cause
This, in 30s<t<In the range of the etch period of 120s, can obtain great surface quality micro-nano structure and height 100nm~
Between 300nm.
A kind of chemical etching that combines that the invention described above is proposed aids in femtosecond laser efficiently controllable processing bulk silicon micro-nano
The method of structure, process principle is as follows：In the case of without mask, directly using Femtosecond-Laser Pulse Excitation in silicon substrate surface, i.e.,
By Femtosecond-Laser Pulse Excitation in the monocrystalline silicon surface of 100 crystal orientation in the present embodiment, due to the characteristic such as femtosecond laser is ultrafast, superpower,
The chemical characteristic of the free electron density redistribution influence machined material that material internal is excited in laser action process, makes
Obtain machined material and amorphous silicon state is changed into by monocrystalline silicon state after laser action, chemism drastically declines.Because of processing district
Domain and the difference of undressed regional chemistry activity, cause the etch rate during chemical etching to differ greatly, so that super
Low chemically active partial operation region serves etch mask effect in etching process, and undressed region is acute with KOH solution
Strong reaction, machining area is relatively low with KOH reaction rates, negligible, ultimately forms large-area high-quality micro-nano structure, realizes
High efficiency processing without mask.
Because the present embodiment is under the conditions of pulse femtosecond laser, to use " flight time punch method " to process large area high
Quality nano-dot matrix array structure.Understood according to the process principle of " flight time punch method ", the repetition rate of femtosecond laser is determined
When the process velocity of nano dot, i.e. repetition rate are 200Hz, nano dot process velocity is 200/second.In sextuple precision surface plate
In the case that translational speed is allowed, increase femtosecond laser repetition rate can then increase nano dot process velocity, further improve
Large area processing efficiency.Additionally, compared to traditional method for increasing mask layer auxiliary etch in material surface, the present invention is proposed
Be a kind of processing method without mask, i.e., using femtosecond laser controlled material chemical property, allow machining area to possess etching and cover
The effect of film layer, therefore, it is possible to save the process of processing mask layer, reduces processing cost, simplifies process and improves
Overall processing efficiency, is to realize large area, the processing method a kind of simple, efficiently, practical of high quality silicon micro-nano structure.
In order to illustrate present disclosure and implementation, this specification gives a specific embodiment.In embodiment
The middle purpose for introducing details is not the scope for limiting claims, and is to aid in understanding the method for the invention.This area
Technical staff should be understood that：Do not departing from the present invention and its spirit and scope of the appended claims, to most preferred embodiment step
Various modifications, change or replacement be all possible.Therefore, the present invention should not be limited to disclosed in most preferred embodiment and accompanying drawing
Content.
Claims (6)
1. it is a kind of efficiently controllable processing bulk silicon micro-nano structure method, it is characterised in that comprise the following steps：
Step one, femtosecond laser beam is focused on using microcobjective；
Step 2, adjusts laser energy：Using half-wave plate-polarizer combination regulation laser energy so that pulsed laser energy is low
Can be continuously adjusted in the ablation threshold on rapidoprint surface, and pulsed laser energy；
Step 3, rapidoprint is fixed on a mobile platform, and regulation mobile platform makes femto-second laser pulse focus on processing material
Material surface；
Step 4, utilizes " flight time punch method ", realizes the large area highly-efficient processing under the conditions of femtosecond laser pulse；
Step 5, the chemical solution that the rapidoprint after femtosecond laser processing in step 4 is placed under the certain concentration of constant temperature
In, after etched time t, obtain that surface is smooth and uniform high quality silicon micro-nano structure.
2. it is according to claim 1 it is a kind of efficiently controllable processing bulk silicon micro-nano structure method, it is characterised in that：Institute
State micro-nano structure including but not limited to class annular silicon column structure, flat-top shape silicon column structure and silicon nano dots structure.
3. it is according to claim 1 it is a kind of efficiently controllable processing bulk silicon micro-nano structure method, it is characterised in that：It is logical
Crossing control laser flux, etch period can be met the different-shape of use requirement and the micro-nano structure of size, and
The spacing of adjacent structure can be controlled by controlling pulse laser repetition rate, sweep speed.
4. it is according to claim 1 it is a kind of efficiently controllable processing bulk silicon micro-nano structure method, it is characterised in that：Step
Rapidoprint described in rapid three is that the N-type of 100 crystal orientation undopes monocrystalline silicon.
5. it is according to claim 1 it is a kind of efficiently controllable processing bulk silicon micro-nano structure method, it is characterised in that：Step
Chemical solution described in rapid five is alkaline solution.
6. according to a kind of method of any described efficiently controllable processing bulk silicon micro-nano structures of claim 1-5, its feature
It is：Chemical solution described in step 5 is the potassium hydroxide solution of concentration 25wt%, and temperature is 55 DEG C, and etch period t is between 30s
To between 120s.
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| CN113130305A (en) * | 2021-03-03 | 2021-07-16 | 哈尔滨工业大学 | Method for constructing surface microstructure of silicon carbide single crystal |
| CN113130305B (en) * | 2021-03-03 | 2023-03-24 | 哈尔滨工业大学 | Method for constructing surface microstructure of silicon carbide single crystal |
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| CN114346446A (en) * | 2022-01-07 | 2022-04-15 | 珠海东辉半导体装备有限公司 | System and method for removing cathode material under screen |
| CN116102238A (en) * | 2022-11-25 | 2023-05-12 | 中国工程物理研究院激光聚变研究中心 | Processing method of fused quartz micro-nano optical device |
| CN116102238B (en) * | 2022-11-25 | 2023-09-26 | 中国工程物理研究院激光聚变研究中心 | Processing method of fused quartz micro-nano optical device |
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