CN110171801A - The preparation method of glass and the alternately arranged self-organizing periodicity micro-nano structure of crystal - Google Patents
The preparation method of glass and the alternately arranged self-organizing periodicity micro-nano structure of crystal Download PDFInfo
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- CN110171801A CN110171801A CN201910400943.6A CN201910400943A CN110171801A CN 110171801 A CN110171801 A CN 110171801A CN 201910400943 A CN201910400943 A CN 201910400943A CN 110171801 A CN110171801 A CN 110171801A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/03—Observing, e.g. monitoring, the workpiece
- B23K26/032—Observing, e.g. monitoring, the workpiece using optical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
- B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
- B23K26/0643—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms comprising mirrors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
- B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
- B23K26/0652—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms comprising prisms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/08—Devices involving relative movement between laser beam and workpiece
- B23K26/082—Scanning systems, i.e. devices involving movement of the laser beam relative to the laser head
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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
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- 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
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00031—Regular or irregular arrays of nanoscale structures, e.g. etch mask layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- 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
- B81C1/005—Bulk micromachining
- B81C1/00515—Bulk micromachining techniques not provided for in B81C1/00507
Abstract
The invention discloses the preparation methods of a kind of glass and the alternately arranged self-organizing periodicity micro-nano structure of crystal.Sample, the sample TERNARY GLASS 35La are prepared using suspension method2O3‑xTa2O5‑(65‑x)Nb2O5(5 < x < 45) or 35La2O3‑xTiO2‑(65‑x)Nb2O5(30 < x < 60), wherein x indicates molar percentage (mol.%)；Sample is fixed on displacement platform, ultrafast laser issues ultrafast laser beam, and ultrafast laser beam is irradiated on sample through shutter, Glan-Taylor prism and half-wave plate, and focuses on sample interior；When sample visible light is occurred by ultrafast laser Shu Jifa at focusing, starts displacement platform, so that sample is taken exercises according to the path and kinematic parameter of setting relative to laser beam, the periodical micro-nano structure of inductive formation polarization independent at the focusing of laser beam.The present invention realizes a kind of high efficiency preparation of the periodical micro-nano structure of polarization independent, has expanded the functional material that can be used for periodical forming Micro-Nano structure.
Description
Technical field
The present invention relates to ultrafast laser technical field of micro and nano fabrication, in particular to a kind of glass and crystal are alternately arranged certainly
Organize the preparation method of periodical micro-nano structure.
Background technique
Ultrafast laser micro-nano technology technology is a kind of minimum using pulsewidth, the high laser pulse progress precision of peak energy
The advanced manufacturing technology of micro-nano technology.The technology mainly passes through the interaction of high field laser and substance, induces a series of physical
Chemical reaction, while is broken through by optical diffraction limit, finally realizes characteristic size for the non-linear absorption of ultrafast pulse using material
Reach nanoscale ultra-precise optical micro Process.
Periodical micro-nano structure has widely in numerous areas such as optical communication, optical storage, light regulation and surface enhanceds
Using, and have great potentiality to be exploited in following quantum calculation, quantum communications field.However periodical micro-nanos most of at present
Structure can only all be generated in material surface, and the periodical micro-nano structure type inside transparent medium is single, and processing efficiency is lower, be fitted
The dielectric material for closing the internal micro-nano periodic structure of preparation is very limited (still based on quartz glass), it is difficult to adapt to micro-nano photon
The functionalization of device, integrated and increasingly increased complexity demand.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of glass is alternately arranged with crystal
Self-organizing periodicity micro-nano structure preparation method, realize a kind of high efficiency system of the periodical micro-nano structure of polarization independent
It is standby, expand the functional material that can be used for periodical forming Micro-Nano structure.
To achieve the goals above, present invention process with the following method:
S1: sample, the sample TERNARY GLASS 35La are prepared using suspension method2O3-xTa2O5-(65-x)Nb2O5(5 < x
< 45) or 35La2O3-xTiO2-(65-x)Nb2O5(30 < x < 60), wherein x indicates molar percentage (mol.%)；
S2: sample is fixed on displacement platform, ultrafast laser issue ultrafast laser beam, ultrafast laser beam through shutter,
Glan-Taylor prism and half-wave plate are irradiated on sample, and focus on sample interior；
S3: allow laser beam static illumination sample for a period of time, when discovery focusing at sample by ultrafast laser Shu Jifa occur
When visible light, is there is infrared light by ultrafast laser Shu Jifa and gradually becomes visible light again in sample at focusing when starting irradiation, then
Start displacement platform, so that sample is taken exercises according to the path and kinematic parameter of setting relative to laser beam, in the focusing of laser beam
Locate the periodical micro-nano structure of inductive formation polarization independent.
Controlled by the shutter in light path system laser by with blocking, pass through Glan Taylor's rib in light path system
Mirror and half-wave plate control the polarization direction of laser beam, by the optical attenuator in light path system by the mean power tune of laser beam
Whole is 150-300mW.
Displacement platform drives sample to do flat scanning movement, so that laser beam is at the focusing of sample interior relative to laser
Beam does flat scanning movement.
The periodical micro-nano structure of different motion generation different patterns is done by displacement platform drive sample.
Using ultrafast laser micro-nano technology manufacture system, ultrafast laser micro-nano technology manufacture system includes computer, ultrafast
Laser, shutter, Glan-Taylor prism, half-wave plate, optical attenuator, the first total reflection mirror, the second total reflection mirror, dichroscope,
Object lens, sample, displacement platform, microscope illuminator, the first polarizing film, the second polarizing film, eyepiece and CCD camera；Ultrafast laser
Output ultrafast laser Shu Yici the first total reflection is incident on after shutter, Glan-Taylor prism, half-wave plate, optical attenuator
Mirror, then successively sample is irradiated to by object lens after the successively reflection of the first total reflection mirror, the second total reflection mirror and dichroscope
And focus on sample interior；Sample fixation is placed on displacement platform, and microscope illuminator is located at below sample, and microscope illuminator is upward
Issue visible light beam, it is seen that light beam is incident on sample through the first polarizing film, visible light beam and ultrafast laser Shu Zhao through sample
It is mapped to the visible light that sample excitation goes out to transmit through dichroscope together, be then successively incident on after the second polarizing film, eyepiece again
CCD camera is detected to be received；Simultaneous computer respectively with ultrafast laser, shutter, displacement platform, CCD camera control port
Connection.
The sample is fixed on displacement platform by fixture.
The polarization direction of first polarizing film and the second polarizing film is perpendicular, by the first polarizing film and the second polarizing film
Constitute cross polarization piece.
The self-organizing periodicity micro-nano structure is preparing the application in infrared optical attenuator.
The invention has the following beneficial effects:
When preparing sample 11, by Ta2O5And TiO2It is added to La2O3-Nb2O5In glass system, La is made2O3-Ta2O5-
Nb2O5Glass and La2O3-TiO2-Nb2O5Glass, due to the introducing of Ta and Ti element, so that the ability of sample 11 greatly enhances,
Allow La2O3-Nb2O5Glass system has the ability for generating periodical micro-nano structure.The addition of Ta and Ti element can also change
Kind La2O3-Nb2O5The thermal stability of glass system improves refractive index, while reducing dispersion.
The present invention realizes self-organizing micro-nano structure using the non-linear process that ultrafast laser and matter interaction cause
Preparation, therefore the preparation process can break through diffraction limit, realize photoelectric elements, greatly improve the forming essence of micro-structure
Degree.
The present invention induces La using ultrafast laser2O3-Ta2O5-Nb2O5And La2O3-TiO2-Nb2O5Inside glass is selectively analysed
Crystalline substance, and glass and the alternately arranged periodical micro-nano structure of crystal are formed using interference field, this micro-nano structure is that self-organizing is raw
At, do not need the complicated motion path of design, it is only necessary to which displacement platform 12 does simple linear motion, greatlies simplify
Manufacture craft.
The present invention can change incident laser by adjusting Glan-Taylor prism 4 in light path system and half-wave plate 5
Polarization direction, and then change the slow axis orientation of self-organizing periodicity micro-nano structure, the external control of micro-nano structure is realized, it is this
Characteristic has potential application in optical storage.
The present invention is for the first time in La2O3-Ta2O5-Nb2O5And La2O3-TiO2-Nb2O5Inside glass generates glass and crystal is handed over
For the polarization independent micro-nano structure being arranged to make up, the preparation for future feature micro element provides new material and new process.
The resulting micro-nano structure of the present invention can be used for making the miniature optical attenuator of infrared band.Attenuator size can be with
Accomplish diameter 2mm hereinafter, size can reduce 50 times or more compared with the plated film attenuator of current maturation.The attenuator is close red
The highest attenuation rate of wave section (800-1550nm) can further promote attenuation rate by multilayer processing up to 60%.
Resulting glass-crystal periodic arrangement the micro-structure of the present invention, physicochemical properties are stablized, are able to bear 870 DEG C of high temperature, can use
In the decaying (irradiation of 6W femtosecond laser can be born at present) of high intensity laser beam.Simultaneously as the structural generation is in glass matrix
Insensitive, the optical signal prosessing that can be used under adverse circumstances is polluted inside to extraneous corrosion.
Detailed description of the invention
Fig. 1 is overall composition schematic diagram of the invention.
Fig. 2 is light path system schematic diagram in Fig. 1.
Fig. 3 is microscopic observation system schematic diagram in Fig. 1.
Fig. 4 is glass and the alternately arranged self-organizing periodicity micro-nano structure preparation process schematic diagram of crystal.
Fig. 5 is attenuator internal structure and working method schematic diagram
In figure: computer 1, ultrafast laser 2, shutter 3, Glan-Taylor prism 4, half-wave plate 5, optical attenuator 6, first are complete
Reflecting mirror 7, the second total reflection mirror 8, dichroscope 9, object lens 10, sample 11, displacement platform 12, microscope illuminator 13, first are inclined
Shake piece 14, the second polarizing film 15, eyepiece 16, CCD camera 17, self-organizing periodicity micro-nano structure 18, ultrafast laser beam 19, laser
Device 20, attenuator 21, power meter 22.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples.
The preparation of periodical micro-nano structure of the invention is realized using a kind of ultrafast laser micro-nano technology manufacture system.Such as figure
Shown in 1, ultrafast laser micro-nano technology manufacture system includes computer, ultrafast laser, light path system, microscopic observation system and position
Move platform.Ultrafast laser is connect with computer, is controlled by computer, for exporting specific laser pulse；Light path system with
Ultrafast laser coupling, focuses on sample interior for ultrafast laser；Microscopic observation system is connect with computer, for observing sample
State and process；Displacement platform is connect with computer, is controlled by computer, for realizing the three-dimensional motion of sample.It is ultrafast
Laser micro/nano fabricates system under control of the computer, irradiates sample by the laser pulse of ultrafast laser output certain parameter
Inside product, while sample does the relative motion of special parameter under the drive of displacement platform, can be in inside glass inductive formation
Glass and the alternately arranged self-organizing periodicity micro-nano structure of crystal.
As shown in Figure 1, present invention specific implementation uses ultrafast laser micro-nano technology manufacture system, ultrafast laser micro-nano technology
Manufacture system includes that computer 1, ultrafast laser 2, shutter 3, Glan-Taylor prism 4, half-wave plate 5, optical attenuator 6, first are complete
Reflecting mirror 7, the second total reflection mirror 8, dichroscope 9, object lens 10, sample 11, displacement platform 12, microscope illuminator 13, first are inclined
Vibration piece 14, the second polarizing film 15, eyepiece 16 and CCD camera 17；The output ultrafast laser Shu Yici of ultrafast laser 2 passes through shutter
3, be incident on the first total reflection mirror 7 after Glan-Taylor prism 4, half-wave plate 5, optical attenuator 6, then successively through the first total reflection mirror 7,
It is irradiated to sample 11 by object lens 10 after the successively reflection of second total reflection mirror 8 and dichroscope 9 and focuses on inside sample 11；
The fixation of sample 11 is placed on displacement platform 12, and sample 11 is fixed on displacement platform 12 by fixture, and microscope illuminator 13 is located at
11 lower section of sample, microscope illuminator 13 issue visible light beam upwards, it is seen that light beam is incident on sample 11 through the first polarizing film 14, thoroughly
The visible light beam and ultrafast laser beam for crossing sample 11 are irradiated to the visible light that sample 11 inspires and transmit together through dichroscope 9,
Then the detected reception of CCD camera 17 is successively incident on after the second polarizing film 15, eyepiece 16 again；Simultaneous computer 1 respectively with
The control port connection of ultrafast laser 2, shutter 3, displacement platform 12, CCD camera 17, is realized by computer 1 to ultrafast laser
Device 2 issues the control of the laser parameter of ultrafast laser beam, the control that shutter 3 is opened and closed, the motion control of displacement platform 12 and CCD
The acquisition of camera 17 shoots control, and then realizes that the three-dimensional of sample 11 is mobile by displacement platform 12.
The polarization direction of first polarizing film 14 and the second polarizing film 15 is perpendicular, by the first polarizing film 14 and the second polarizing film
15 constitute cross polarization piece.
As shown in Fig. 2, light path system is mainly complete by shutter 3, Glan-Taylor prism 4, half-wave plate 5, optical attenuator 6, first
Reflecting mirror 7, the second total reflection mirror 8, dichroscope 9 and object lens 10 are constituted；The opening and closing of shutter 3 is for controlling ultrafast laser beam 19
By being used for cut-off, Glan-Taylor prism 4 and half-wave plate 5 for controlling the polarization direction of ultrafast laser beam 19, optical attenuator 6
The power of ultrafast laser beam 19 is controlled, total reflection mirror 7-8 is used to for ultrafast laser beam 19 to be oriented to dichroscope 9, and dichroscope 9 is used
Object lens 10 and the simultaneously visible light of transmission sample 11 are imported in reflection ultrafast laser beam 19, are schemed so that microscopic observation system receives
As signal, object lens 10 are realized the induction preparation of micro-nano structure, are collected simultaneously for focusing on ultrafast laser beam inside sample 11
The optical signal of sample 11, so as to microscopic observation system reception.
As shown in figure 3, microscopic observation system is mainly by microscope illuminator 13, the first polarizing film 14, the second polarizing film 15, mesh
Mirror 16 and CCD camera 17 are constituted；Microscope illuminator 13 is located at 11 lower section of sample, upward irradiating sample 11.Microscope illuminator 13 is used
In providing radiation of visible light sample 11 to carry out microexamination, the first polarizing film 14 can as the control sending of microscope illuminator 13
The light-exposed polarizer；Second polarizing film 15 is used as analyzer, since periodical micro-nano structure can be modulated light wave, tool
There are some special optical signatures, such as periodically birefringent, microscopic observation system can also be detected by cross polarization piece 14-15
The birefringent signal of machining area judges whether there is micro-nano structure generation.Object lens 10 are used to collect the visible light of sample 11, two to
Look mirror 9 is used for through visible light, eyepiece 16 and CCD camera 17 for collecting visible light signal, and computer 1 is connected with CCD camera,
Display and processing for micro-image.
The embodiment of the present invention is as follows:
Embodiment 1:
Step 1: sample 11,11 TERNARY GLASS 35La of sample are prepared using suspension method2O3-xTa2O5-(65-x)Nb2O5(5
< x < 45), wherein x indicates molar percentage (mol.%).
Ta is adjusted by setting2O5Or TiO2Molar percentage x, adjust sample 11 crystallization ability, the more big then sample of x
The crystallization ability of product 11 is stronger, and inductive formation micro-nano structure is easier, and the process velocity used is faster, but the preparation of sample 11
It can become more difficult.The Ta of setting is embodied in the present invention2O5Or TiO2Molar percentage x can realize glass well
The preparation of the alternately arranged periodical micro-nano structure of glass-crystal.
Step 2: sample 11 is fixed on displacement platform 12, and the position for being suitble to processing is found by microscopic observation system,
Its xyz triaxial coordinate is determined, in case subsequent setting kinematic parameter.
Step 3: machining path is imported into computer 1, the kinematic parameter of specific machining path are as follows: setting processing speed
1000-4000 μm/s is spent, 30-60 μm of working depth, motion path parameter can also be set when making special pattern, as spiral is transported
Dynamic, reciprocating motion and point-by-point jump etc.；
Step 4: processing laser parameter is imported into computer 1, specific laser parameter are as follows: setting mean power is one
A biggish initial value 3000mW, to guarantee the stability of laser output, pulse width 1-4ps, repetition rate 100-200kHz；
Step 5: starting ultrafast laser 2 makes ultrafast laser beam 19 enter light path system along symmetrical center line, passes through
Shutter 3 in light path system come control ultrafast laser beam 19 by with blocking, pass through the Glan-Taylor prism 4 in light path system
The polarization direction that ultrafast laser beam 19 is controlled with half-wave plate 5, by the optical attenuator 6 in light path system, by ultrafast laser beam
The mean power of 19 actual processings is adjusted to 150-300mW.Ultrafast laser beam 19 passes through the reflecting mirror 7-8 in light path system, with
And dichroscope 9, it is focused on inside sample 11 into object lens 10, and by object lens 10.
Step 6: allowing 11 a period of time of laser beam static illumination sample, when finding that focal zone scattering light enhances suddenly,
When i.e. sample 11 visible light is occurred by the excitation of ultrafast laser beam 19, starts displacement platform 12, make sample 11 according to the path of setting
It takes exercises with kinematic parameter relative to laser beam, the periodical micro-nano of inductive formation polarization independent at the focusing of ultrafast laser beam
Structure 18.
Periodical micro-nano structure is the bar shaped micro-nano structure of the period profile positioned at focussing plane.Such as Fig. 4 in specific implementation
As it can be seen that multiple strip structures are on same focussing plane for the form of multiple strip structure array periods arrangement.
Step 7: laser beam is closed in processing after generating, and the microscope illuminator 13 in microscopic observation system is opened, by micro-
The CCD camera 17 of observing system observes machining area pattern, after processing is completed, rotates two panels polarizing film 14-15, polarizes two panels
The polarization direction of piece is mutually perpendicular to form cross polarization piece.Through CCD camera acquisition image discovery, wherein occur polarization according to
There is the periodical birefringent phenomenon of polarization independent in bad periodical micro-nano structure, this explanation has self-organizing periodicity micro-nano knot
Structure 18 generates, and the specific pattern of the structure is as shown in Figure 4.
Embodiment 2:
Step 1: sample 11,11 TERNARY GLASS 35La of sample are prepared using suspension method2O3-xTiO2-(65-x)Nb2O5(30
< x < 60), wherein x indicates molar percentage (mol.%).
Ta is adjusted by setting2O5Or TiO2Molar percentage x, adjust sample 11 crystallization ability, the more big then sample of x
The crystallization ability of product 11 is stronger, and inductive formation micro-nano structure is easier, and the process velocity used is faster, but the preparation of sample 11
It can become more difficult.The Ta of setting is embodied in the present invention2O5Or TiO2Molar percentage x can realize glass well
The preparation of the alternately arranged periodical micro-nano structure of glass-crystal.
Step 2: sample 11 is fixed on displacement platform 12, and the position for being suitble to processing is found by microscopic observation system,
Its xyz triaxial coordinate is determined, in case subsequent setting kinematic parameter.
Step 3: machining path is imported into computer 1, the kinematic parameter of specific machining path are as follows: setting processing speed
1000-4000 μm/s is spent, 30-60 μm of working depth, motion path parameter can also be set when making special pattern, as spiral is transported
Dynamic, reciprocating motion and point-by-point jump etc.；
Step 4: processing laser parameter is imported into computer 1, specific laser parameter are as follows: setting mean power is one
A biggish initial value 3000mW, to guarantee the stability of laser output, pulse width 1-4ps, repetition rate 100-200kHz；
Step 5: starting ultrafast laser 2 makes ultrafast laser beam 19 enter light path system along symmetrical center line, passes through
Shutter 3 in light path system come control ultrafast laser beam 19 by with blocking, pass through the Glan-Taylor prism 4 in light path system
The polarization direction that ultrafast laser beam 19 is controlled with half-wave plate 5, by the optical attenuator 6 in light path system, by ultrafast laser beam
The mean power of 19 actual processings is adjusted to 150-300mW.Ultrafast laser beam 19 passes through the reflecting mirror 7-8 in light path system, with
And dichroscope 9, it is focused on inside sample 11 into object lens 10, and by object lens 10.
Step 6: 11 a period of time of laser beam static illumination sample is allowed, is occurred when sample 11 is excited by ultrafast laser beam 19
When visible light, starts displacement platform 12, sample 11 is made to take exercises according to the path and kinematic parameter of setting relative to laser beam,
The periodical micro-nano structure 18 of inductive formation polarization independent at the focusing of ultrafast laser beam.
Periodical micro-nano structure is the bar shaped micro-nano structure of the period profile positioned at focussing plane.Such as Fig. 4 in specific implementation
As it can be seen that multiple strip structures are on same focussing plane for the form of multiple strip structure array periods arrangement.
Step 7: laser beam is closed in processing after generating, and the microscope illuminator 13 in microscopic observation system is opened, by micro-
The CCD camera 17 of observing system observes machining area pattern, after processing is completed, rotates two panels polarizing film 14-15, polarizes two panels
The polarization direction of piece is mutually perpendicular to form cross polarization piece.Through CCD camera acquisition image discovery, wherein occur polarization according to
There is the periodical birefringent phenomenon of polarization independent in bad periodical micro-nano structure, this explanation has self-organizing periodicity micro-nano knot
Structure 18 generates, and the specific pattern of the structure is as shown in Figure 4.
Originally due to the setting of cross polarization piece so that the visible light beam that microscope illuminator 13 issues passes through cross polarization piece
It can not penetrate, there is no the Image Acquisition of any light beam at CCD camera；But under technical solution of the present invention, due to glass
The self-organizing periodicity micro-nano structure 18 of interior surface growth can act on visible light beam, its polarization angle is made to deflect,
To penetrate second piece of polarizing film, allow the optical signal appeared that ultrafast laser machining area is collected at CCD camera,
And judge whether micro-nano structure generates with this.
The present invention generates plasma wave in uneven particle or defect and the incident field interaction of inside glass, etc.
Ion bulk wave and the light wave of subsequent input interfere the periodic distribution for leading to distribution of light intensity in focal zone, and then cause to swash
The periodic distribution for sending out plasma density, finally causes the periodic distribution in temperature field.
For machined material 11, the periodic distribution in temperature field will cause the selective crystallization of inside glass, analysis
Crystalline region domain matches with optical interference style, same to have periodically.
Since this crystallization only occurs in the nonlinear ionization region at focal beam spot center, it can break through optics and spread out
Emitter-base bandgap grading limit makes this selective crystallization have nano-scale dimension, and direction depends on the polarization direction of incident laser, determining work
Glass can be formed under skill parameter and crystal is alternately arranged the polarization independent micro-nano structure of composition.
As shown in figure 5, the resulting periodical micro-nano structure of the present invention can be used for making the miniature optical attenuation of infrared band
Device 21.Press 15-20 microns of interval scanning a plurality of self-organizing periodicity micro-nano structures when production at 40 microns below sample surfaces
18, a grating array is constituted, diffraction can occur when the laser that laser 20 issues passes through array of scan lines, wherein zero level is spread out
The power for penetrating spot can generate strong and weak alternate variation with the variation of laser polarization direction, this is because periodical micro-nano structure
Caused by light selective reflecting and absorption to particular polarization, therefore attenuator 21 can play optical attenuation with the size of very little
Effect.
Comparative example:
Work as La2O3-Nb2O5Ta in glass system2O5And TiO2Content it is too low or without when, the crystallization ability of glass is significantly
It reduces, the variations in refractive index of regional area can only be generated under the action of ultrafast laser, it can not inducing periodic crystallization formation rule
The alternate periodical micro-nano structure of crystal-glass then, therefore attenuation can not be generated to optical signal.Work as La2O3-Nb2O5Glass
Ta in glass system2O5And TiO2Too high levels when, ternary system crystallization ability is too strong, becomes ceramics after smelting in suspension, can not be by
Glass, devitrification is made, therefore micro-nano structure can not be processed in inside.
Mature commercialization attenuator carries out optical attenuation using coated reflection principle at present, and this attenuator needs biggish
Size is to guarantee the continuous and even variation of coating film thickness, it is difficult to accomplish miniaturization and integrated.Plated film attenuator can not be held simultaneously
By higher energy input, when decaying for infrared high power laser light is easily damaged.
The present invention is able to achieve the preparation of the periodical micro-nano structure for the decaying of infrared high power laser light, and realizes one
The high efficiency preparation of the periodical micro-nano structure of kind polarization independent, has expanded the function material that can be used for periodical forming Micro-Nano structure
Material.
Claims (9)
1. the preparation method of a kind of glass and the alternately arranged self-organizing periodicity micro-nano structure of crystal, it is characterised in that: method
Process is as follows:
S1: being prepared sample (11) using suspension method, the sample (11) TERNARY GLASS 35La2O3-xTa2O5-(65-x)Nb2O5
(5 < x < 45) or 35La2O3-xTiO2-(65-x)Nb2O5(30 < x < 60), wherein x indicates molar percentage (mol.%)；
S2: sample (11) is fixed on displacement platform (12), and ultrafast laser (2) issues ultrafast laser beam, ultrafast laser beam
It is irradiated on sample (11) through shutter (3), Glan-Taylor prism (4) and half-wave plate (5), and it is internal to focus on sample (11)；
S3: laser beam static illumination sample (11) a period of time is allowed, sample (11) is by ultrafast laser Shu Jifa at discovery focusing
When there is visible light, then start displacement platform (12), makes sample (11) according to the path and kinematic parameter of setting relative to sharp
Light beam is taken exercises, the periodical micro-nano structure of inductive formation polarization independent at the focusing of laser beam.
2. the preparation side of a kind of glass according to claim 1 and the alternately arranged self-organizing periodicity micro-nano structure of crystal
Method, it is characterised in that: controlled by the shutter (3) in light path system laser by with blocking, by light path system
Glan-Taylor prism (4) and half-wave plate (5) control the polarization direction of laser beam, pass through the optical attenuator (6) in light path system
The mean power of laser beam is adjusted to 150-300mW.
3. the preparation side of a kind of glass according to claim 1 and the alternately arranged self-organizing periodicity micro-nano structure of crystal
Method, it is characterised in that: displacement platform (12) drives sample (11) to do flat scanning movement, so that laser beam is internal in sample (11)
Focusing at relative to laser beam do flat scanning movement.
4. the preparation side of a kind of glass according to claim 1 and the alternately arranged self-organizing periodicity micro-nano structure of crystal
Method, it is characterised in that: the periodicity for driving sample (11) to do different motion generation different patterns by displacement platform (12) is micro-
Micro-nano structure.
5. the preparation side of a kind of glass according to claim 1 and the alternately arranged self-organizing periodicity micro-nano structure of crystal
Method, it is characterised in that: use ultrafast laser micro-nano technology manufacture system, ultrafast laser micro-nano technology manufacture system includes computer
(1), ultrafast laser (2), shutter (3), Glan-Taylor prism (4), half-wave plate (5), optical attenuator (6), the first total reflection mirror
(7), the second total reflection mirror (8), dichroscope (9), object lens (10), sample (11), displacement platform (12), microscope illuminator
(13), the first polarizing film (14), the second polarizing film (15), eyepiece (16) and CCD camera (17)；The output of ultrafast laser (2)
It is complete that ultrafast laser Shu Yici is incident on first after shutter (3), Glan-Taylor prism (4), half-wave plate (5), optical attenuator (6)
Reflecting mirror (7), then successively lead to after the successively reflection of the first total reflection mirror (7), the second total reflection mirror (8) and dichroscope (9)
Object lens (10) are crossed to be irradiated to sample (11) and focus on sample (11) inside；Sample (11) fixation is placed on displacement platform (12),
Microscope illuminator (13) is located at below sample (11), and microscope illuminator (13) issues visible light beam upwards, it is seen that light beam is through first
Polarizing film (14) is incident on sample (11), and the visible light beam and ultrafast laser beam through sample (11) are irradiated to sample (11) excitation
Visible light out is transmitted through dichroscope (9) together, is then successively incident on after (16) through the second polarizing film (15), eyepiece again
CCD camera (17) is detected to be received；Simultaneous computer (1) respectively with ultrafast laser (2), shutter (3), displacement platform (12),
The control port of CCD camera (17) connects.
6. the preparation side of a kind of glass according to claim 1 and the alternately arranged self-organizing periodicity micro-nano structure of crystal
Method, it is characterised in that: the sample (11) is fixed on displacement platform (12) by fixture.
7. the preparation side of a kind of glass according to claim 1 and the alternately arranged self-organizing periodicity micro-nano structure of crystal
Method, it is characterised in that: the polarization direction of first polarizing film (14) and the second polarizing film (15) is perpendicular, by the first polarization
Piece (14) and the second polarizing film (15) constitute cross polarization piece.
8. a kind of glass and the alternately arranged self-organizing periodicity micro-nano structure of crystal, it is characterised in that: use claim 1-7
Any the method preparation.
9. the application of glass according to any one of claims 8 and the alternately arranged self-organizing periodicity micro-nano structure of crystal, feature exist
In: the self-organizing periodicity micro-nano structure is preparing the application in infrared optical attenuator.
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| CN113917586A (en) * | 2021-10-18 | 2022-01-11 | 浙江大学 | Micro light splitting element and preparation method thereof |
| CN114734138A (en) * | 2022-04-24 | 2022-07-12 | 中国科学院重庆绿色智能技术研究院 | Method for enhancing laser energy absorption efficiency of spatial additive manufacturing wire |
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| CN110171801B (en) | 2022-01-07 |
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