CN108015410A - One kind is based on femtosecond laser induction amorphous gemSbnTekThe method of film preparation crystalline state nanostructured - Google Patents
One kind is based on femtosecond laser induction amorphous gemSbnTekThe method of film preparation crystalline state nanostructured 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
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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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- 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
One kind is based on femtosecond laser induction amorphous gemSbnTekThe method of film preparation crystalline state nanostructured, belongs to femtosecond laser applied technical field.The present invention realizes Ge by being controlled in certain energy range to single incident femto-second laser pulse focal beam spot sizemSbnTekCrystalline state nano particle is processed and the control of size, when focal beam spot is larger, can obtain larger diameter nano particle, reduces focal beam spot size, can reduce the diameter of nano particle.The control of comprehensive laser frequency and translation stage translational speed can further realize that high uniformity, the large area of uniform crystalline state nano particle are efficiently prepared.Existing nanostructured processing method is contrasted, the present invention effectively increases the machining accuracy and processing efficiency of nanostructured, realizes the controllable preparation of single nanostructured and composite nanostructure, while realize ultrafast phase-change material GemSbnTekThe change of nanostructured crystalline nature, has vital application value in information storage and Meta Materials, nano-antenna and photocontrol etc..
Description
Technical field
The present invention relates to femtosecond laser to induce amorphous gemSbnTekThe method of film preparation crystalline state nanostructured, belongs to winged
Second laser application technique field.
Background technology
Ultrafast laser and its minute manufacturing have the uniqueness ultrafast, superpower, 3 D super precision is close compared with traditional long pulse
Property, is one of forward position of contemporary minute manufacturing method.As one kind of ultrafast laser, three characteristics of femtosecond laser so that
Femtosecond laser micro-nano technology has unique advantage.Micro Nano material has a variety of excellent performances, in optics, photoelectronics,
Before the fields such as photonic propulsion, plasma, photo-biological sensing, micro-nano fluid, micro-fluidic optical, biomedicine have far-reaching application
Scape.In these areas, surface micronano technology can change the optical property of material, mechanicalness as a kind of effective method
Energy, chemical property, wetability and other many performances.The minute manufacturing of femtosecond laser surface has become a novelty and effective
Process for treating surface, can process the micro-nano structure of different shape in the surface of solids, be widely used in photoelectron, bio-sensing, micro-
Receive fluid, biological medicine etc..Control and manipulation of the micro/nano-scale to light are the primary study objects of modern age optical research.Especially
It, when structure size as low as nanometer scale, the atom of body structure surface can quantitatively compare with internal atom, so in table
The electronics in face produces skin effect, is limited and produces be subject to structure size plus the electronics mean free path of inside configuration
Dimensional effect, the optical characteristics that nanostructured is shown are very different with block materials.In the range of sub-wavelength, metal is received
Rice structure (nano-pillar, nanotip, nano particle etc.) shows stronger electron excitation and collective's concussion (local surfaces etc.
Gas ions) stronger resonance response (localized surface plasmons resonance) can be produced to light.To the form of metal Nano structure
Carrying out regulation and control can couple with optomagnetic field component, it can be achieved that the control of optical property and the preparation of negative index element.So
And metal causes larger absorption and fuel factor in optical frequency range in the presence of higher ohmic loss, it is limited in light
Application on electronics.Electrolyte/nanometer semiconductor structure with high index can also realize the tune of light in nanoscale
Control and manipulation.According to Mie theory, due to the resonance effects of high index of refraction electrolyte nano structure so that electrolyte nano
Structure also is used as Meta Materials, realizes negative magnetoconductivity and dielectric constant.Ultrafast phase-change material can be in amorphous state and crystalline state
Between change, the characteristic such as the optics of both states and electricity has larger difference, make its data store and remember on have
Have wide practical use.GemSbnTekWith preferable heat endurance, it is a kind of typical ultrafast phase-change material, makees in laser
With the phase co-conversion between lower achievable amorphous state and crystalline state.The crystalline state GeSbTe nanostructureds of ordered arrangement greatly change
The characteristics such as its optics, electricity, can be widely applied in photonic propulsion, photoelectronics, infrared source and Photobiology device, have huge
Big application and potentiality to be exploited.A difficult point and hot spot for current nanometer manufacture, regular at present during the processing of surface nano-structure
Prepared by the nanostructured of arrangement usually requires appendage acquisition, prepared by such as substrate template or mask.In the recent period, in document
“Laser fabrication of crystalline siliconanoresonators from an amorphous
In filmfor low-loss all-dielectric nanophotonics ", Dmitriev et al. is by using big umber of pulse
(tens thousand of, 104) femtosecond laser direct write induction amorphous silicon film wetting removal effect, is used to prepare crystalline state silicon nanostructure.But
This processing method is excessive to processing platform precise requirements to be used for smaller laser direct-writing wire cutting, and excessive laser pulse number
Processing efficiency is limited, it is constrained and is widely applied.
The content of the invention
It is an object of the present invention to provide one kind based on femtosecond laser induction amorphous gemSbnTekFilm preparation crystalline state nano junction
The method of structure, to overcome currently available technology above shortcomings.
Idea of the invention is that being distributed pulse femtosecond laser beam by using normal Gaussian, go to moisten based on film surface
The phase transition process of wet effect and ultrafast phase-change material under laser action, realizes crystalline state GemSbnTekThe efficient of nanostructured can
Control processing and ordered arrangement.Using femto-second laser pulse material surface ablation threshold effect so that be deposited on film
Active region material surface is cut into two regions by pulse energy so that center be cut material and polar region surface produce every
From heat transfer effect, central role region material under the action of surface tension to center convergence formed nanostructured, at the same time
Under the interaction of laser and material, the amorphous ge that is appliedmSbnTekUndergo phase transition, be changed into crystalline state from amorphous.
The purpose of the present invention is what is be achieved through the following technical solutions：
One kind is based on femtosecond laser induction amorphous gemSbnTekThe method of film preparation crystalline state nanostructured, its feature exist
In：Comprise the following steps：
Step 1, sample preparation：Different-thickness amorphous ge is carried out in selected substrate surfacemSbmTekFilm processing；
Step 2, processed sample is fixed on sextuple translation stage, using focusing objective len to incident femto-second laser pulse
It is focused, adjusts femtosecond laser processing light path, it is ensured that laser light incident direction is perpendicular to sample surface；
Step 3, energy adjustment：Cause incident femto-second laser pulse using half-wave plate-polarizer combination and continuous attenuator
Energy is continuously adjustable, by being imaged the observation of CCD, adjusts incident laser energy and is higher than film single pulse ablation threshold value, and incident
Laser energy is less than 1.5Fth, FthFor single pulse ablation threshold value；So that the laser action regional center of material produces ablation；
Step 4, comprehensive fs-laser system pulse frequency and the control of mechanical switch opening time so that single laser
Pulsed irradiation point pulse number is 1；
Step 5, respectively under the conditions of the different processing object lens conditions of fixed thickness and fixed processing object lens difference thickness,
Nanostructured, which produces, finds single femto-second laser pulse induction amorphous ge in energy rangemSbnTekFilm preparation crystalline state nano junction
The processing rule of structure；
Step 6, the single femto-second laser pulse induction crystalline state Ge found according to step 5mSbnTekThe processing of nanostructured
Rule, film thickness, pulse energy and focusing objective len with reference to needed for required processing nano-structure morphology selection, is processed.
The sample of specific thickness is processed, can by select that different focusing objective lens realizes focal beam spot size
Adjust, so that the size of film ablated area under the laser action that gaussian-shape is distributed is adjustable.Energy is produced in nanostructured
In the range of, select 20 object lens, 10 object lens, 5 object lens and focal length to be processed for 100mm planoconvex spotlights to sample successively, so that
The Characteristic Distribution of crystalline state nanostructured is processed under the conditions of to different focusing objective lens, draws nano junction under different processing object lens
Structure diameter distribution curve figure (D).
Processing crystalline state nano structure under the conditions of the difference focusing objective len is：Process the higher (focusing of object lens multiple
Apart from smaller), the crystalline state nanostructure diameter processed is smaller；The crystalline state nanostructured processed using 20 object lens
Diameter it is minimum, the diameter maximum for the crystalline state nanostructured that focal length is processed by 100mm planoconvex spotlights.Each processing object lens
The nanostructure diameter D that particular range size is corresponded in energy range is produced in nanostructured.
Fixed processing object lens, select different thickness films to be processed；For different thickness conditions, pass through the continuous of energy
Adjust, determine energy (F) scope a≤F≤b prepared by crystalline state nanostructured；Pressed for certain films thick quilt processing sample from energy a
It is sequentially increased according to corresponding step-length to energy b and processes nano particle in film surface, different size of nanostructured is obtained, by setting
Surely amount is spaced in sample surface and processes diameter (D) into monotonic increase curve distribution nanostructured.
Producing crystalline state nano structure under the conditions of the difference film thickness is：With the increase of thickness, nanometer is produced
Energy range gradually increases needed for structure；Under the conditions of specific thickness, with the increase of pulse energy, the size of gained nanostructured
Monotone decreasing；With the increase of thickness, the nanostructured size of generation gradually increases, and each energy value corresponds to a D value.
Preferably, by being programmed to the sextuple mobile platform mobile process, to adjacent two laser exposure spots
Position is controlled, and can obtain evenly arranged nano-pillar lattice structure.
Preferably, processing object lens 20 × processing of selection object lens, 10 × processing object lens, 5 × processing object lens and the focal length
For 100mm planoconvex spotlights.
Preferably, described carry out plating Ge in processed sample surfacemSbnTekThe method that film process uses magnetron sputtering,
Thickness range is 20nm~70nm.
Preferably, processed sample choice of the substrates silicon, silica or the SOI materials.
Beneficial effect
The present invention proposes a kind of based on femtosecond laser induction amorphous gemSbnTekFilm preparation crystalline state nanostructured
Method, ablation effect is produced by pulse gaussian-shape femtosecond laser on the membrane surface, is imitated in thin-film material wetting removal
Under the action of answering, the processing generation nanostructured in substrate samples.Meanwhile the omnidirectional Ge under laser actionmSbnTekProduce phase
Become, be changed into crystalline structure.Comprehensive laser irradiation hot spot, film thickness and machining energy are cut the big ditty of material by adjusting
Material Local Instantaneous state is controlled, the induction that accurately can realize substrate surface nanostructured according to advance design produces.It is meanwhile comprehensive
The control of laser frequency and laser direct-writing speed is closed, substantially increases the machining accuracy and processing efficiency of surface nano-structure, can
Realize any arrangement, greatly promote application of the ultrafast phase-change material in terms of information storage, meanwhile, in Meta Materials and light tune
Control etc. also has vital application value.
Brief description of the drawings
Fig. 1 is femtosecond laser induction amorphous ge in specific embodimentmSbnTekFilm preparation crystalline state nanostructured is processed
Index path：
Fig. 2 be specific embodiment in gaussian-shape femto-second laser pulse cut thin-film material surface so that be cut material with
Surrounding films material and substrate samples produce thermal isolation, and material, which occurs, to center shifts to form nanostructured machining sketch chart：
Label：1- femto-second lasers；2- half-wave plates；3- polarizers；4- speculums；The continuous attenuators of 5-；6- a quarters
Wave plate；7- mechanical switch；8- dichroscopes；9- illuminates white light source；10- beam splitters；11- planoconvex spotlights；12- is imaged CCD；13-
Process object lens；14- samples to be processed；15- 6 DOF mobile platforms.
Embodiment
Below in conjunction with the accompanying drawings and embodiment is described further the present invention.
In present embodiment, amorphous ge is induced using pulse femtosecond lasermSbnTekFilm preparation crystalline state nanostructured
Method, specific processing light path are as shown in Figure 1.It is processed light path and produces femto-second laser pulse, femtosecond laser arteries and veins for femto-second laser 1
Punching is after half-wave plate 2, polarizer 3, through continuous attenuator 5 after being reflected by speculum 4, quarter-wave plate 6, and mechanical switch, 7
Afterwards, 14 surface of sample is focused on after being reflected by dichroscope 8 after processing object lens 13, sample 14 to be processed is fixed on sextuple shifting
On moving platform 15；Illumination white light source 9 is irradiated to 14 back reflection light of sample after beam splitter 10, dichroscope 8, processing object lens 13
Processed object lens 13, dichroscope 8, are incided in imaging CCD12 by beam splitter reflection 10 after planoconvex spotlight 11.
The femto-second laser parameter used in experimentation is as follows：Centre wavelength is 800nm, pulse width 35fs, is weighed
Complex frequency is 1kHz, linear polarization；Sample to be processed is the amorphous ge that different-thickness is deposited with substrate in experimentmSbnTekIt is thin
Film.
Femto-second laser 1 is using the laser of U.S.'s spectrum physics (Spectrum Physics) company production, laser wave
Long 800nm, pulse width 35fs, repetition rate 1KHz, pulse ceiling capacity 3mJ, light distribution are gaussian-shape, linear polarization.
Continuous attenuator 5 is using Daheng's photoelectricity GCC-3030 circle neutral density gradual filters, in visible ray to infrared
The ratio of absorption/reflection light and transmitted light by adjusting the rotation angle of eyeglass, can be changed in light area to change the big of optical attenuation
Small, laser energy adjustable range is 1% -90%.
Mechanical switch 7 can control Laser exposure dwell times, when it switchs response using the SH05 of Thorlabs companies production
Between be 1ms.
Embodiment：
To process crystalline state Ge2Sb2Te5Exemplified by nano-grain array, pulse femtosecond using the present invention swashs processing method,
Used femto-second laser pulse is linear polarization, and specific procedure of processing is as follows：
Adjust light path, it is ensured that laser light incident direction is vertical with processed sample surface；
(1) sample preparation：The present embodiment is by the method for magnetron sputtering on the monocrystalline silicon sample of 10mm × 10mm × 1mm
Plate 50nmGe2Sb2Te5Film (film thickness adjustable extent is 20nm~70nm), GemSbnTekM, n and k value can pass through magnetic control
Sputtering target material control is different values.
(2) energy is adjusted：Combined using half-wave plate 2- polarizers 3 and continuous attenuator 5 adjusts laser energy and is allowed to be more than
The single pulse ablation threshold value on sample material surface is processed, and laser energy can continuously adjust；
(3) femto-second laser pulse is focused using 20 × object lens 13, processed sample 14 is fixed on sextuple mobile flat
On platform 15, by being imaged the observation of CCD11, sextuple mobile platform 15 is adjusted so that femto-second laser pulse focuses on 13 table of sample
Face；
(4) it is 10Hz to adjust 1 pulse frequency of fs-laser system, and holding mechanical switch 7 is always-on, is controlled sextuple flat
Moving stage moves 15 50 μm/s of speed, so that the pulse number of each laser exposure spots is 1；
(5) sextuple 15 mobile process of mobile platform is programmed, adjacent two direct writes line spacing is 5 μm, be can obtain uniformly
Arrangement transverse direction and longitudinal direction spacing is 5 μm of two-dimensional array arrangement nanostructured.
Embodiment 2：
To process crystalline state Ge2Sb2Te5Exemplified by nano-grain array, pulse femtosecond using the present invention swashs processing method,
Used femto-second laser pulse is circular polarization state, and specific procedure of processing is as follows：
Other steps are same as Example 1, and difference is：Add in the optical path before the progress of step (2) energy adjustment
Enter quarter-wave plate 6, adjust quarter-wave plate 6 so that 45 ° of wave plate optical axis direction and former laser polarization direction angle so as to
Obtain circular polarization 800nm femto-second laser pulses.It is processed under the conditions of circular polarization state femto-second laser pulse.
Embodiment 1,2 comparative results：
Since under the action of laser polarity, surface forms structure and produces class plasma effect, the table of generation is excited
Surface plasma field is radially distributed, material under more uniform stress to center convergence, therefore in embodiment 2 using circle
Polarize the crystalline state Ge of femto-second laser pulse processing2Sb2Te5Nanoparticle structure is not flexible, and form is more preferable.
Above-described specific descriptions, have carried out further specifically the purpose, technical solution and beneficial effect of invention
It is bright, it should be understood that the foregoing is merely the specific embodiment of the present invention, the protection model being not intended to limit the present invention
Enclose, within the spirit and principles of the invention, any modification, equivalent substitution, improvement and etc. done, should be included in the present invention
Protection domain within.
Claims (5)
1. one kind is based on femtosecond laser induction amorphous gemSbnTekThe method of film preparation crystalline state nanostructured, its feature exist
In：Comprise the following steps：
Step 1, sample preparation：Different-thickness amorphous ge is carried out in selected substrate surfacemSbmTekFilm processing；
Step 2, processed sample is fixed on sextuple translation stage, and incident femto-second laser pulse is carried out using focusing objective len
Focus on, adjust femtosecond laser processing light path, it is ensured that laser light incident direction is perpendicular to sample surface；
Step 3, energy adjustment：Cause incident femto-second laser pulse energy using half-wave plate-polarizer combination and continuous attenuator
It is continuously adjustable, by being imaged the observation of CCD, adjust incident laser energy and be higher than film single pulse ablation threshold value, and incident laser
Energy is less than 1.5Fth, FthFor single pulse ablation threshold value；So that the laser action regional center of material produces ablation；
Step 4, comprehensive fs-laser system pulse frequency and the control of mechanical switch opening time so that single laser pulse
Exposure spots pulse number is 1；
Step 5, respectively under the conditions of the different processing object lens conditions of fixed thickness and fixed processing object lens difference thickness, in nanometer
Structure, which produces, finds single femto-second laser pulse induction amorphous ge in energy rangemSbnTekFilm preparation crystalline state nanostructured
Process rule；
Step 6, the single femto-second laser pulse induction crystalline state Ge found according to step 5mSbnTekThe processing rule of nanostructured
Rule, film thickness, pulse energy and focusing objective len with reference to needed for required processing nano-structure morphology selection, is processed.
It is 2. according to claim 1 a kind of based on femtosecond laser induction amorphous gemSbnTekFilm preparation crystalline state nano junction
The method of structure, it is characterised in that：According to the speed of required two adjacent nanostructures spacing size Comprehensive Control 6 DOF translation stage and
Fs-laser system frequency, obtains the adjustable nanostructured arbitrary arrangement of spacing.
It is 3. according to claim 1 a kind of based on femtosecond laser induction amorphous gemSbnTekFilm preparation crystalline state nano junction
The method of structure, it is characterised in that：Amorphous ge is deposited in selected substrate surfacemSbnTekFilm process is using magnetron sputtering
Method, thickness range are 20nm~70nm, m, n, and the selection of k values is controlled by target material composition used in magnetron sputtering.
It is 4. according to claim 1 a kind of based on femtosecond laser induction amorphous gemSbnTekFilm preparation crystalline state nano junction
The method of structure, it is characterised in that described to find single femto-second laser pulse induction amorphous gemSbnTekFilm preparation crystalline state nanometer
The specific method of structure processing rule is as follows：
(1) by selecting different focusing objective lens to be processed the form of control crystalline state nanostructured：
The sample of specific thickness is processed, by selecting different focusing objective lens to realize the adjustable of focal beam spot size, from
And make it that the size of film ablated area under the laser action that gaussian-shape is distributed is adjustable；Certain energy size is kept, is selected successively
Select 20 × object lens, 10 × object lens, 5 × object lens and focal length to be processed sample for 100mm planoconvex spotlights, so as to obtain different poly-
The Characteristic Distribution of crystalline state nanostructured is processed under the conditions of focus objective lens；
Processing crystalline state nano structure under the conditions of the difference focusing objective len is：Process the higher i.e. focusing distance of object lens multiple
Smaller, the crystalline state nanostructure diameter processed is smaller；The crystalline state nanostructured processed using 20 × object lens
Diameter is minimum, and the diameter for the crystalline state nanostructured that focal length is processed by 100mm planoconvex spotlights is maximum；
(2) the processing form of nanostructured is controlled by the selection of film thickness：
Object lens are processed according to determined by (one), select different thickness films to be processed；For different thickness conditions, pass through energy
Amount continuously adjusts, and determines energy (F) scope a≤F≤b prepared by crystalline state nanostructured；Sample is processed for certain films thick quilt
It is sequentially increased from energy a according to corresponding step-length to energy b and processes nano particle in film surface, obtains different size of nanometer
Structure；The machined material of different thickness produces in energy range in nanostructured and produces different size of crystalline state GemSbnTekIt is brilliant
State nano particle；
Producing crystalline state nano structure under the conditions of the difference film thickness is：With the increase of thickness, nanostructured is produced
Required energy range gradually increases；Under the conditions of specific thickness, with the increase of pulse energy, the size of gained nanostructured is dull
Successively decrease；With the increase of thickness, the nanostructured size of generation gradually increases.
It is 5. according to claim 1 a kind of based on femtosecond laser induction amorphous gemSbnTekFilm preparation crystalline state nano junction
The method of structure, it is characterised in that：The crystalline state GemSbnTekThe generation of nanostructured is to be higher than ablation single pulse ablation threshold
Under the gaussian-shape femto-second laser pulse effect of value, the circular cutting of ablation is produced on the membrane surface higher than ablation threshold region, from
And make it that center material to be cut and substrate surface heat transfer completely cut off, heartcut material under the action of wetting removal effect to
Center convergence forms nano particle.
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