CN109954987A - A method of nanometer blind hole is processed on single-silk surface using femtosecond laser - Google Patents
A method of nanometer blind hole is processed on single-silk surface using femtosecond laser Download PDFInfo
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- CN109954987A CN109954987A CN201910233029.7A CN201910233029A CN109954987A CN 109954987 A CN109954987 A CN 109954987A CN 201910233029 A CN201910233029 A CN 201910233029A CN 109954987 A CN109954987 A CN 109954987A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention proposes a kind of using femtosecond laser in the method for single-silk surface processing nanometer blind hole, belongs to femtosecond laser application field.Femto-second laser pulse sequence is focused on silk surface by lens or micro objective first by this method, by regulating and controlling to be incident on femto-second laser pulse number, flux of energy and the polarization direction on silk surface, self-existent single oval nanometer blind hole has been prepared on silk surface.Principle of the method for the present invention based near field light modulation realizes and is much smaller than the single nanometer blind hole of diffraction limit in the processing of silk surface.It is compared with the traditional method, the advantage that the present invention has machining accuracy high, flexible and convenient provides a kind of feasible method to prepare high sensor.
Description
Technical field
The present invention relates to a kind of using femtosecond laser in the method for single-silk surface processing nanometer blind hole, belongs to femtosecond and swashs
Light applied technical field.
Background technique
Silk is a kind of ancient biomaterial, is applied together with the nature materials such as cotton, animal skin by the mankind
It thousand, since silk has special structure type, excellent mechanical property, is had important application in textile industry.In addition,
There are good optical lens due to fibroin with excellent biocompatibility and in the visible light wave range of 400nm~700nm
Performance is penetrated, the photoelectric sensor for organism monitoring is can be used as and is taken seriously.For example, silk has been applied to tooth bacterium
Sensor, edible fruit maturity monitoring sensor etc..
The realization of above-mentioned device is processed firstly the need of to silk.Currently, the processing method of fibroin device is main
It is to obtain pure silk fibroin protein solution by carrying out the processes such as degumming, dialysis to natural silk cocoon, further passes through casting, rotation again
Painting, Soft lithograph, nano impression, ink jet printing etc. obtain the structure with corresponding function.But since silk size itself is small by (~10
μm) and mechanical property it is strong, it is extremely difficult that micro-nano technology is directly carried out to natural silk.
Summary of the invention
The purpose of the present invention is to propose to a kind of method using femtosecond laser in single-silk surface processing nanometer blind hole, needles
To the current method for lacking and processing nanometer blind hole directly on single-silk, during femtosecond laser and Effect of Silk Fibroin
Beam modulation near field principle and Multi-photon Nonlinear sink effect, by Reasonable Regulation And Control femtosecond laser parameter, generate it is self-existent,
Minor axis length is less than the oval blind hole structure of 100nm.
The method proposed by the present invention for processing nanometer blind hole on silk surface using femtosecond laser, comprising the following steps:
(1) ablation threshold of silk to be processed is measured using epitaxy, process is as follows:
N number of flux of energy is F by (1-1)0Femto-second laser pulse by lens focus arrive silk surface, according to incidence
Femtosecond laser wavelength X, spot diameter DL, factor of quality M2Focal point waist radius ω is calculated with focal length of lens f0,
The silk ablated surface round spot radius r that (1-2) measuring process (1-1) obtains;
(1-3) calculates silk ablation threshold F under N number of pulseth,
(2) femto-second laser pulse sequence is focused on into single-silk surface by lens or micro objective;
(3) parameter of femtosecond laser is controlled are as follows: femto-second laser pulse number is 300~800, and the energy of femtosecond laser is logical
Amount is 1.05~1.15 times of silk ablation threshold under corresponding pulses number, and the polarization direction of femtosecond laser and silk axially hang down
Directly, it processes to obtain self-existent nanometer ellipse blind hole on silk surface.
The method specific steps of above-mentioned silk surface processing nanometer blind hole are as follows:
(2-1) constructs a femtosecond laser system of processing, including femto-second laser, half-wave plate, neutral density attenuator, electricity
Control shutter, lighting source, semi-transparent semi-reflecting lens, dichroscope, lens or microcobjective and translation stage;The femto-second laser hair
Femtosecond laser out passes sequentially through half-wave plate, neutral density attenuator and automatically controlled shutter and forms the first optical path, the illumination light
The visible light that source issues, which passes sequentially through semi-transparent semi-reflecting lens, dichroscope, lens or microcobjective and is irradiated on translation stage, forms the
Two optical paths, the charge coupled cell and imaging len form third optical path;First optical path and the second optical path is mutual
Vertically, and at dichroscope intersect, second optical path is mutually perpendicular to third optical path, and the phase at semi-transparent semi-reflecting lens
It hands over;
(2-2) debugs femtosecond laser system of processing: opening femto-second laser, generates femto-second laser pulse, turn down
Repetition rate sets automatically controlled shutter as single exposure mode, sets the time for exposure, make the femtosecond laser arteries and veins by shutter to 10Hz
Rushing number is 1, adjusts the height of translation stage, and the ablation round spot diameter for generating single pulse under fixed energies on silk surface is most
It is small, the debugging of femtosecond laser system of processing is completed, femtosecond laser is correctly focused on silk surface at this time;
(2-3) adjusts the polarization direction of femto-second laser pulse by half-wave plate, and irradiation is made to arrive the femtosecond laser on silk surface
Pulse polarization direction is vertical with silk axis direction.
(2-4) makes the single pulse energy flux for being incident on silk surface correspond to arteries and veins by adjusting neutral density attenuator
It rushes between 1.05~1.15 times of silk ablation threshold under number;
The time for exposure of femto-second laser repetition rate and automatically controlled shutter is arranged in (2-5), makes the femtosecond laser by shutter
Umber of pulse is N, completes processing.The purpose of the present invention is what is realized by following technology:
A kind of method using femtosecond laser in single-silk surface processing nanometer blind hole proposed by the present invention, advantage
It is:
1, preparing after silk protein aqueous solution through casting, spin coating, Soft lithograph, nanometer in the method for the present invention and prior art
The comparison of the methods of coining, ink jet printing, femtosecond laser minute manufacturing method of the invention are a kind of processing non-contact, without exposure mask
Method, has the characteristics that ultrafast, superpower, high-precision, directly can prepare highly sensitive Protein sensor using natural silk.
2, the method for the present invention has determined that the single pulse energy flux for being incident on silk surface is silk under respective pulses number
, it can be achieved that prepared by oval blind hole of the self-existent, minor axis length less than 100nm at 1.05~1.15 times of ablation threshold, add
Work precision is high.
3, the surface of the method for the present invention processing preparation is machined with the silk of nano-pore, using femtosecond laser, directly to single
Natural silk is processed, and has many advantages, such as simple process, and flexibility is good.
Detailed description of the invention
Fig. 1 is the femtosecond laser system of processing used in the embodiment of the present invention.
In Fig. 1,1 is femto-second laser, and 2 be half-wave plate, and 3 be neutral density attenuator, and 4 be automatically controlled shutter, and 5 be illumination light
Source, 6 be semi-transparent semi-reflecting lens, and 7 be dichroscope, and 8 be lens or microcobjective, and 9 be silk, and 10 be translation stage, and 11 be charge coupling
It closes element (CCD), 12 be imaging len.
Specific embodiment
The method proposed by the present invention for processing nanometer blind hole on silk surface using femtosecond laser, comprising the following steps:
(1) ablation threshold of silk to be processed is measured using epitaxy, process is as follows:
N number of flux of energy is F by (1-1)0Femto-second laser pulse by lens focus arrive silk surface, according to incidence
Femtosecond laser wavelength X, spot diameter DL, factor of quality M2Focal point waist radius ω is calculated with focal length of lens f0,
The silk ablated surface round spot radius r that (1-2) measuring process (1-1) obtains;
(1-3) calculates silk ablation threshold F under N number of pulseth,
(2) femto-second laser pulse sequence is focused on into single-silk surface by lens or micro objective;
(3) parameter of femtosecond laser is controlled are as follows: femto-second laser pulse number is 300~800, and the energy of femtosecond laser is logical
Amount is 1.05~1.15 times of silk ablation threshold under corresponding pulses number, and the polarization direction of femtosecond laser and silk axially hang down
Directly, it processes to obtain self-existent nanometer ellipse blind hole on silk surface.
The method of processing nanometer blind hole in silk surface proposed by the present invention, specifically:
(2-1) constructs a femtosecond laser system of processing, and structure is as shown in Figure 1, include femto-second laser 1, half-wave plate
2, neutral density attenuator 3, automatically controlled shutter 4, lighting source 5, semi-transparent semi-reflecting lens 6,8 and of dichroscope 7, lens or microcobjective
Translation stage 10;The femtosecond laser that the femto-second laser 1 issues passes sequentially through half-wave plate 2, neutral density attenuator 3 and automatically controlled
Shutter 4 forms the first optical path, and the visible light that the lighting source 5 issues passes sequentially through semi-transparent semi-reflecting lens 6, dichroscope 7, thoroughly
Mirror or microcobjective 8, which are irradiated on translation stage 10, forms the second optical path, 12 shape of the charge coupled cell 11 and imaging len
At third optical path;First optical path is mutually perpendicular to the second optical path, and is intersected at dichroscope 7, second light
Road is mutually perpendicular to third optical path, and is intersected at semi-transparent semi-reflecting lens 6;
(2-2) debugs femtosecond laser system of processing: opening femto-second laser 1, generates femto-second laser pulse, turn down
For repetition rate to 10Hz, setting automatically controlled shutter 4 is single exposure mode, sets the time for exposure, makes the femtosecond laser by shutter
Umber of pulse is 1, adjusts the height of translation stage 10, and the ablation round spot for generating the single pulse under fixed energies on silk surface is straight
Diameter is minimum, completes the debugging of femtosecond laser system of processing, femtosecond laser is correctly focused on 9 surface of silk at this time;
(2-3) adjusts the polarization direction of femto-second laser pulse by half-wave plate 2, swashs irradiation to the femtosecond on 9 surface of silk
Light pulse polarization direction is vertical with silk axis direction.
(2-4) corresponds to the single pulse energy flux for being incident on 9 surface of silk by adjusting neutral density attenuator 3
Under pulse number between 1.05~1.15 times of silk ablation threshold;
The time for exposure of femto-second laser repetition rate and automatically controlled shutter 4 is arranged in (2-5), makes the femtosecond laser by shutter
Umber of pulse is N number of, completion processing.
With reference to the accompanying drawing and embodiment is described further the present invention:
The present invention is implemented in femtosecond laser system of processing as shown in Figure 1, which includes processing subsystem and observation
Subsystem two parts.Wherein processing subsystem include femto-second laser 1, half-wave plate 2, neutral density attenuator 3, automatically controlled shutter 4,
Dichroscope 7, lens or microcobjective 8 and translation stage 10.Observing subsystem includes lighting source 5, semi-transparent semi-reflecting lens 6, lens
Or microcobjective 8, charge coupled cell (CCD) 11 and imaging len 12.
In processing subsystem, the femto-second laser pulse sequence of femto-second laser output successively penetrates half-wave plate 2 and adjusts partially
Vibration direction, neutral density attenuator 3 are reflected by dichroscope 7 after adjusting energy, and focus on silk through lens or microcobjective 8
9 surfaces.Wherein, automatically controlled shutter 4 is equipped between neutral density attenuator 3 and dichroscope 7, for accuracy controlling irradiation to silk
The pulse number on 9 surfaces.Silk 9 is fixed on translation stage 10, for accurately controlling the position of processed nanometer blind hole.Implement
The parameter of femto-second laser 1 in example are as follows: femtosecond laser central wavelength 800nm, repetition rate 1Hz~1kHz is adjustable, pulse width
For 35fs.
In observation subsystem, the illumination light that lighting source 5 issues after semi-transparent semi-reflecting lens 6 and dichroscope 7 transmit by
Lens or microcobjective 8 focus on 9 surface of silk for illuminating to machining area.The realtime graphic of machining area is through lens
Or dichroscope 7 is penetrated after the amplification of microcobjective 8, then be reflected into imaging len 12 by semi-transparent semi-reflecting lens 6.Imaging len 12 is used
It is processed for observing in amplified realtime graphic is imaged on charge coupled cell (CCD) 11 and is transmitted to display
Journey.
The method that the present invention processes nanometer blind hole on silk surface using femtosecond laser, comprising the following steps:
Femto-second laser pulse sequence is focused on silk surface by lens or micro objective by step 1.Step 1 tool
Body includes:
Step 1.1) opens femto-second laser 1, generates femto-second laser pulse.Polarization direction is adjusted by half-wave plate 2, is made
The polarization direction that 9 surface of silk must be irradiated is vertical with silk axis direction.
Step 1.2) makes the single pulse energy flux pair for being incident on 9 surface of silk by adjusting neutral density attenuator 3
1.05~1.15 times for answering silk ablation threshold under pulse number.
Step 2 realizes the processing of nano-pore using local near field light modulation principle by regulation femtosecond laser parameter.
Step 2 specifically includes:
Step 2.1) selectes lens or microcobjective 8, silk 9 is fixed on translation stage 10, adjusts lens or micro- object
The relative position of 10 working face of mirror 8 and translation stage makes to focus on 9 surface of silk by the femtosecond laser of lens or microcobjective 8
At specified Working position.
Step 2.2) controls spoke by coordinating the single exposure time of regulation femtosecond laser repetition rate and automatically controlled shutter 4
The pulse train number N on silk 9 is shone, processing is completed.
It is less than 100nm's in the nano-pore that silk surface is formed using the method for the present invention for self-existent, minor axis length
Oval blind hole.
It is the embodiment of the method for the present invention below:
Embodiment 1:
Neutral density attenuator 3 is adjusted, setting single pulse energy is 48.7nJ (4.34J/cm2, 1.13Fth);Setting is saturating
Mirror or microcobjective 8 are 50 × long reach flat field semi-apochromat (NA=0.5);By automatically controlled shutter 4, spoke is controlled
Shining the pulse train number N on silk 9 is 350.It is 74nm's that self-existent, minor axis length is prepared on silk 9
Oval blind hole.
Embodiment 2:
Neutral density attenuator 3 is adjusted, setting single pulse energy is 43.1nJ (3.84J/cm2, 1.07Fth);Setting is saturating
Mirror or microcobjective 8 are 50 × long reach flat field semi-apochromat (NA=0.5);By automatically controlled shutter 4, spoke is controlled
Shining the pulse train number N on silk 9 is 450.It is 22nm's that self-existent, minor axis length is prepared on silk 9
Oval blind hole.
Embodiment 3:
Neutral density attenuator 3 is adjusted, setting single pulse energy is 40.1nJ (3.58J/cm2, 1.06Fth);Setting is saturating
Mirror or microcobjective 8 are 50 × long reach flat field semi-apochromat (NA=0.5);By automatically controlled shutter 4, spoke is controlled
Shining the pulse train number N on silk 9 is 650.It is 66nm's that self-existent, minor axis length is prepared on silk 9
Oval blind hole.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (2)
1. it is a kind of using femtosecond laser single-silk surface processing nanometer blind hole method, it is characterised in that: this method includes
Following steps:
(1) ablation threshold of silk to be processed is measured using epitaxy, process is as follows:
N number of flux of energy is F by (1-1)0Femto-second laser pulse by lens focus arrive silk surface, according to incidence femtosecond
Laser wavelength lambda, spot diameter DL, factor of quality M2Focal point waist radius ω is calculated with focal length of lens f0,
The silk ablated surface round spot radius r that (1-2) measuring process (1-1) obtains;
(1-3) calculates silk ablation threshold F under N number of pulseth,
(2) femto-second laser pulse sequence is focused on into single-silk surface by lens or micro objective;
(3) parameter of femtosecond laser is controlled are as follows: femto-second laser pulse number is 300~800, and the flux of energy of femtosecond laser is
1.05~1.15 times of silk ablation threshold under corresponding pulses number, the polarization direction of femtosecond laser and silk are axially vertical,
Silk surface processes to obtain self-existent nanometer elliptical aperture.
2. the method for processing nanometer blind hole in silk surface as described in claim 1, it is characterised in that this method includes following step
It is rapid:
(2-1) constructs a femtosecond laser system of processing, including femto-second laser, half-wave plate, neutral density attenuator, automatically controlled fast
Door, lighting source, semi-transparent semi-reflecting lens, dichroscope, lens or microcobjective and translation stage;What the femto-second laser issued
Femtosecond laser passes sequentially through half-wave plate, neutral density attenuator and automatically controlled shutter and forms the first optical path, the lighting source hair
Visible light out, which passes sequentially through semi-transparent semi-reflecting lens, dichroscope, lens or microcobjective and is irradiated on translation stage, forms the second light
Road, the charge coupled cell and imaging len form third optical path;First optical path is mutually perpendicular to the second optical path,
And intersect at dichroscope, second optical path is mutually perpendicular to third optical path, and is intersected at semi-transparent semi-reflecting lens;
(2-2) debugs femtosecond laser system of processing: opening femto-second laser, generates femto-second laser pulse, turn down repetition
Frequency sets automatically controlled shutter as single exposure mode, sets the time for exposure, make the femto-second laser pulse number by shutter to 10Hz
It is 1, adjusts the height of translation stage, the ablation round spot diameter for generating the single pulse under fixed energies on silk surface is minimum,
The debugging of femtosecond laser system of processing is completed, femtosecond laser is correctly focused on silk surface at this time;
(2-3) adjusts the polarization direction of femto-second laser pulse by half-wave plate, and irradiation is made to arrive the femto-second laser pulse on silk surface
Polarization direction is vertical with silk axis direction.
(2-4) makes the single pulse energy flux respective pulses for being incident on silk surface by adjusting neutral density attenuator
Between 1.05~1.15 times of several lower silk ablation thresholds;
The time for exposure of femto-second laser repetition rate and automatically controlled shutter is arranged in (2-5), makes the femto-second laser pulse by shutter
Number is N, completes processing.
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CN110640307A (en) * | 2019-09-18 | 2020-01-03 | 清华大学 | Functional ceramic welding device based on time domain shaping femtosecond laser |
CN110695515A (en) * | 2019-09-18 | 2020-01-17 | 清华大学 | Method and system for processing nanocone array on silk film by femtosecond laser |
CN111375902A (en) * | 2020-04-13 | 2020-07-07 | 中国航空制造技术研究院 | Laser processing pinhole device based on scanning galvanometer |
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