CN110171801B - Preparation method of self-organized periodic micro-nano structure with alternately arranged glass and crystals - Google Patents
Preparation method of self-organized periodic micro-nano structure with alternately arranged glass and crystals Download PDFInfo
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- 230000000737 periodic effect Effects 0.000 title claims abstract description 66
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- 239000013078 crystal Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006073 displacement reaction Methods 0.000 claims abstract description 33
- 230000010287 polarization Effects 0.000 claims abstract description 29
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000033001 locomotion Effects 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
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- 239000000725 suspension Substances 0.000 claims abstract description 6
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- 230000001939 inductive effect Effects 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 239000008204 material by function Substances 0.000 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000007514 turning Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
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- 238000000576 coating method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
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- 238000010956 selective crystallization Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000005355 lead glass Substances 0.000 description 1
- 238000005459 micromachining Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 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
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- 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
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- 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
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Abstract
The invention discloses a preparation method of a self-organized periodic micro-nano structure with alternately arranged glass and crystals. Preparing a sample by using a suspension method, wherein the sample is ternary glass 35La2O3‑xTa2O5‑(65‑x)Nb2O5(5 < x < 45) or 35La2O3‑xTiO2‑(65‑x)Nb2O5(30 < x < 60), wherein x represents the mole percentage (mol.%); fixing a sample on a displacement platform, wherein an ultrafast laser emits an ultrafast laser beam, and the ultrafast laser beam irradiates the sample through a shutter, a Glan Taylor prism and a half-wave plate and is focused into the sample; when a sample at a focusing position is excited by an ultrafast laser beam to generate visible light, a displacement platform is started, so that the sample moves relative to the laser beam according to a set path and a set motion parameter, and a polarization-dependent periodic micro-nano structure is induced and generated at the focusing position of the laser beam. The invention realizes the high-efficiency preparation of the polarization-dependent periodic micro-nano structure and expands the functional materials for forming the periodic micro-nano structure.
Description
Technical Field
The invention relates to the technical field of ultrafast laser micro-nano processing, in particular to a preparation method of a self-organized periodic micro-nano structure with alternately arranged glass and crystals.
Background
The ultrafast laser micro-nano processing technology is an advanced manufacturing technology for performing precise micro-nano processing by utilizing laser pulses with extremely small pulse width and extremely high peak energy. The technology induces a series of physical and chemical reactions mainly through the interaction of strong field laser and substances, simultaneously utilizes nonlinear absorption of materials to ultrafast pulses, breaks through the limit of optical diffraction, and finally realizes the ultraprecise optical micromachining with characteristic dimension reaching the nanometer level.
The periodic micro-nano structure has wide application in various fields such as optical communication, optical storage, optical modulation and control, surface enhancement and the like, and has great development potential in the fields of future quantum computation and quantum communication. However, most of the conventional periodic micro-nano structures can only be generated on the surface of a substance, the type of the periodic micro-nano structures in the transparent medium is single, the processing efficiency is low, the medium material suitable for preparing the internal micro-nano periodic structures is very limited (mainly quartz glass), and the requirements on functionalization, integration and increasing complexity of micro-nano photonic devices are difficult to adapt.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a self-organized periodic micro-nano structure with alternately arranged glass and crystals, so that the high-efficiency preparation of a polarization-dependent periodic micro-nano structure is realized, and functional materials for forming the periodic micro-nano structure are expanded.
In order to achieve the purpose, the invention adopts the following method processes:
s1: preparing a sample by using a suspension method, wherein the sample is ternary glass 35La2O3-xTa2O5-(65-x)Nb2O5(5 < x < 45) or 35La2O3-xTiO2-(65-x)Nb2O5(30 < x < 60), wherein x represents the mole percentage (mol.%);
s2: fixing a sample on a displacement platform, wherein an ultrafast laser emits an ultrafast laser beam, and the ultrafast laser beam irradiates the sample through a shutter, a Glan Taylor prism and a half-wave plate and is focused into the sample;
s3: and (3) allowing a laser beam to statically irradiate the sample for a period of time, when the sample at the focusing position is excited by the ultrafast laser beam to generate visible light, starting irradiation, wherein the sample at the focusing position is excited by the ultrafast laser beam to generate infrared light and then gradually change the infrared light into the visible light, starting the displacement platform to enable the sample to move relative to the laser beam according to a set path and movement parameters, and inducing the focusing position of the laser beam to generate a polarization-dependent periodic micro-nano structure.
The passing and the blocking of the laser are controlled by a shutter in the optical path system, the polarization direction of the laser beam is controlled by a Glan Taylor prism and a half-wave plate in the optical path system, and the average power of the laser beam is adjusted to 150-300mW by an optical attenuator in the optical path system.
The displacement platform drives the sample to do plane scanning movement, so that the laser beam does plane scanning movement relative to the laser beam at the focusing position inside the sample.
The displacement platform drives the sample to do different motions to generate periodic micro-nano structures with different patterns.
An ultrafast laser micro-nano processing and manufacturing system is adopted, and comprises a computer, an ultrafast laser, a shutter, a Glan Taylor prism, a half-wave plate, an optical attenuator, a first total reflector, a second total reflector, a dichroic mirror, an objective lens, a sample, a displacement platform, a micro illuminator, a first polaroid, a second polaroid, an eyepiece and a CCD camera; an output ultrafast laser beam of the ultrafast laser sequentially passes through a shutter, a Glan Taylor prism, a half-wave plate and an optical attenuator and then is incident to a first total reflector, and then sequentially reflects the output ultrafast laser beam through the first total reflector, a second total reflector and a dichroic mirror, and then irradiates a sample through an objective lens and focuses the sample inside; the sample is fixedly arranged on the displacement platform, the microscopic illuminator is positioned below the sample, the microscopic illuminator upwards emits a visible light beam, the visible light beam is incident to the sample through the first polaroid, the visible light beam penetrating through the sample and the visible light excited by the ultrafast laser beam irradiating on the sample are transmitted through the dichroic mirror together, and then the visible light beam is incident to the CCD camera after sequentially passing through the second polaroid and the ocular lens to be detected and received; and simultaneously, the computer is respectively connected with the ultrafast laser, the shutter, the displacement platform and the control port of the CCD camera.
The sample is fixed on the displacement platform through a clamp.
The polarization directions of the first polarizer and the second polarizer are perpendicular, and the first polarizer and the second polarizer form a crossed polarizer.
The self-organized periodic micro-nano structure is applied to the preparation of infrared optical attenuators.
The invention has the following beneficial effects:
in preparing sample 11, Ta2O5And TiO2Is added to La2O3-Nb2O5In a glass system, La is produced2O3-Ta2O5-Nb2O5Glass and La2O3-TiO2-Nb2O5Glass, due to the introduction of Ta and Ti elements, the capability of sample 11 is greatly enhanced, and La is allowed2O3-Nb2O5The glass system has the capability of generating a periodic micro-nano structure. Ta and Ti are added, and La can be improved2O3-Nb2O5The thermal stability of the glass system improves the refractive index and reduces the dispersion.
The invention realizes the preparation of the self-organizing micro-nano structure by utilizing the nonlinear process caused by the interaction of the ultrafast laser and the substance, so the preparation process can break through the diffraction limit, realize the nano-scale processing and greatly improve the forming precision of the microstructure.
The invention utilizes ultrafast laser to induce La2O3-Ta2O5-Nb2O5And La2O3-TiO2-Nb2O5The interior of the glass is selectively crystallized, and an interference field is utilized to form a periodic micro-nano structure with alternately arranged glass and crystals, the micro-nano structure is generated by self-organization, a complex motion path is not required to be designed, and only the displacement platform 12 is required to do simple linear motion, so that the manufacturing process is greatly simplified.
The polarization direction of incident laser can be changed by adjusting the Glan Taylor prism 4 and the half-wave plate 5 in the optical path system, so that the slow axis orientation of the self-organized periodic micro-nano structure is changed, the external control of the micro-nano structure is realized, and the characteristic has potential application in optical storage.
The invention is firstly at La2O3-Ta2O5-Nb2O5And La2O3-TiO2-Nb2O5The glass is formed by alternately arranging glass and crystals insideThe polarization of the micro-nano structure is dependent on the micro-nano structure, and a new material and a new process are provided for the preparation of future functional micro devices.
The micro-nano structure obtained by the invention can be used for manufacturing a micro optical attenuator of an infrared band. The size of the attenuator can be less than 2mm in diameter, and compared with the existing mature coated attenuator, the size of the attenuator can be reduced by more than 50 times. The maximum attenuation rate of the attenuator in the near infrared band (800-. The glass-crystal periodic arrangement microstructure obtained by the invention has stable physical and chemical properties, can bear 870 ℃ high temperature, and can be used for attenuation of high-intensity laser (can bear 6W femtosecond laser irradiation at present). Meanwhile, the structure is generated in the glass substrate, so that the structure is insensitive to external corrosion and pollution and can be used for optical signal processing in severe environment.
Drawings
Fig. 1 is a schematic view of the overall constitution of the present invention.
Fig. 2 is a schematic diagram of the optical path system of fig. 1.
FIG. 3 is a schematic view of the microscopic observation system of FIG. 1.
FIG. 4 is a schematic diagram of a process for preparing a self-organized periodic micro-nano structure with alternately arranged glass and crystals.
FIG. 5 is a schematic diagram of the internal structure and operation of the attenuator
In the figure: the system comprises a computer 1, an ultrafast laser 2, a shutter 3, a Glan Taylor prism 4, a half-wave plate 5, an optical attenuator 6, a first total reflecting mirror 7, a second total reflecting mirror 8, a dichroic mirror 9, an objective lens 10, a sample 11, a displacement platform 12, a micro illuminator 13, a first polaroid 14, a second polaroid 15, an ocular lens 16, a CCD camera 17, a self-organized periodic micro-nano structure 18, an ultrafast laser beam 19, a laser 20, an attenuator 21 and a power meter 22.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
The preparation of the periodic micro-nano structure is realized by using an ultrafast laser micro-nano processing and manufacturing system. As shown in fig. 1, the ultrafast laser micro-nano processing and manufacturing system includes a computer, an ultrafast laser, a light path system, a microscopic observation system and a displacement platform. The ultrafast laser is connected with the computer, is controlled by the computer and is used for outputting specific laser pulses; the optical path system is coupled with the ultrafast laser to focus the ultrafast laser into the sample; the microscopic observation system is connected with the computer and is used for observing the state and the processing process of the sample; the displacement platform is connected with the computer and controlled by the computer, and is used for realizing the three-dimensional movement of the sample. The ultrafast laser micro-nano processing and manufacturing system is controlled by a computer, a laser pulse with certain parameters is output by an ultrafast laser to irradiate the inside of a sample, and meanwhile, the sample is driven by a displacement platform to make relative motion with specific parameters, so that a self-organized periodic micro-nano structure with alternately arranged glass and crystals can be induced and generated in the glass.
As shown in fig. 1, the ultrafast laser micro-nano processing and manufacturing system is adopted in the specific implementation of the present invention, and comprises a computer 1, an ultrafast laser 2, a shutter 3, a glan taylor prism 4, a half-wave plate 5, an optical attenuator 6, a first total reflector 7, a second total reflector 8, a dichroic mirror 9, an objective lens 10, a sample 11, a displacement platform 12, a micro-illuminator 13, a first polarizing film 14, a second polarizing film 15, an eyepiece 16 and a CCD camera 17; an ultrafast laser beam output by the ultrafast laser 2 sequentially passes through a shutter 3, a Glan Taylor prism 4, a half-wave plate 5 and an optical attenuator 6, then enters a first total reflector 7, sequentially reflects by the first total reflector 7, a second total reflector 8 and a dichroic mirror 9, then irradiates a sample 11 through an objective lens 10 and focuses inside the sample 11; the sample 11 is fixedly arranged on a displacement platform 12, the sample 11 is fixed on the displacement platform 12 through a clamp, a microscopic illuminator 13 is positioned below the sample 11, the microscopic illuminator 13 emits a visible light beam upwards, the visible light beam is incident on the sample 11 through a first polaroid 14, the visible light beam penetrating through the sample 11 and the visible light excited by the ultrafast laser beam irradiating on the sample 11 are transmitted through a dichroic mirror 9, then sequentially pass through a second polaroid 15 and an ocular 16 and then are incident on a CCD camera 17 to be detected and received; meanwhile, the computer 1 is respectively connected with the ultrafast laser 2, the shutter 3, the displacement platform 12 and the control port of the CCD camera 17, the computer 1 controls the laser parameters of the ultrafast laser beam emitted by the ultrafast laser 2, the opening and closing of the shutter 3, the motion control of the displacement platform 12 and the acquisition and shooting control of the CCD camera 17, and then the three-dimensional movement of the sample 11 is realized through the displacement platform 12.
The polarization directions of the first polarizing plate 14 and the second polarizing plate 15 are perpendicular to each other, and the first polarizing plate 14 and the second polarizing plate 15 constitute crossed polarizing plates.
As shown in fig. 2, the optical path system is mainly composed of a shutter 3, a glan-taylor prism 4, a half-wave plate 5, an optical attenuator 6, a first total reflection mirror 7, a second total reflection mirror 8, a dichroic mirror 9, and an objective lens 10; the device comprises a shutter 3, a Glan Taylor prism 4, a half-wave plate 5, a dichroic mirror 9, an objective lens 10 and a micro-nano structure, wherein the shutter 3 is opened and closed to control the passing and stopping of an ultrafast laser beam 19, the Glan Taylor prism 4 and the half-wave plate 5 are used to control the polarization direction of the ultrafast laser beam 19, an optical attenuator 6 is used to control the power of the ultrafast laser beam 19, total reflection mirrors 7-8 are used to guide the ultrafast laser beam 19 to the dichroic mirror 9, the dichroic mirror 9 is used to reflect the ultrafast laser beam 19 and guide the ultrafast laser beam into the objective lens 10 and transmit visible light of a sample 11 at the same time so that a micro-observation system can receive image signals, and the objective lens 10 is used to focus the ultrafast laser beam into the sample 11, so that the micro-nano structure can be induced and prepared, and optical signals of the sample 11 can be collected so that the micro-observation system can receive the optical signals.
As shown in fig. 3, the microscopic observation system is mainly composed of a microscopic illuminator 13, a first polarizing plate 14, a second polarizing plate 15, an eyepiece 16, and a CCD camera 17; the microscopic illuminator 13 is located below the sample 11 and irradiates the sample 11 upward. The micro-illuminator 13 is used for providing visible light to irradiate the sample 11 so as to carry out microscopic observation, and the first polaroid 14 is used as a polarizer for controlling the micro-illuminator 13 to emit the visible light; the second polarizer 15 is used as an analyzer, and the periodic micro-nano structure can modulate light waves, so that the periodic micro-nano structure has some special optical characteristics, such as periodic birefringence, and the microscopic observation system can also detect a birefringence signal of a processing area through the crossed polarizers 14-15 to judge whether the micro-nano structure is generated. The objective lens 10 is used for collecting visible light of the sample 11, the dichroic mirror 9 is used for passing through the visible light, the ocular lens 16 and the CCD camera 17 are used for collecting visible light signals, and the computer 1 is connected with the CCD camera and used for displaying and processing microscopic images.
The embodiment of the invention is as follows:
example 1:
the method comprises the following steps: sample 11 was prepared by the suspension method, sample 11 being 35La ternary glass2O3-xTa2O5-(65-x)Nb2O5(5 < x < 45), where x represents the mole percentage (mol.%).
By setting to adjust Ta2O5Or TiO2The larger x is, the stronger the crystallization ability of the sample 11 is, the easier the micro-nano structure is induced to be generated, and the faster the processing speed is used, but the more difficult the preparation of the sample 11 becomes. Ta of an embodiment of the invention2O5Or TiO2The preparation of the periodic micro-nano structure with the glass-crystal alternate arrangement can be well realized by the molar percentage x.
Step two: fixing the sample 11 on a displacement platform 12, finding a position suitable for processing through a microscopic observation system, and determining the xyz three-axis coordinates of the sample for setting motion parameters subsequently.
Step three: the machining path is imported into the computer 1, and the motion parameters of the specific machining path are as follows: setting the processing speed of 1000-;
step four: the processing laser parameters are led into the computer 1, and the specific laser parameters are as follows: setting the average power as a larger initial value of 3000mW to ensure the stability of laser output, the pulse width of 1-4ps and the repetition frequency of 100-200 kHz;
step five: the ultrafast laser 2 is started to make the ultrafast laser beam 19 enter the optical path system along the symmetrical central line, the passing and blocking of the ultrafast laser beam 19 are controlled by the shutter 3 in the optical path system, the polarization direction of the ultrafast laser beam 19 is controlled by the Glan Taylor prism 4 and the half-wave plate 5 in the optical path system, and the average power actually processed by the ultrafast laser beam 19 is adjusted to 150-300mW by the optical attenuator 6 in the optical path system. The ultrafast laser beam 19 passes through the mirrors 7 to 8 in the optical path system, and the dichroic mirror 9, enters the objective lens 10, and is focused inside the sample 11 through the objective lens 10.
Step six: and (3) statically irradiating the sample 11 by using a laser beam for a period of time, and starting the displacement platform 12 when the scattered light of a focusing area is suddenly enhanced, namely the sample 11 is excited by the ultrafast laser beam 19 to generate visible light, so that the sample 11 moves relative to the laser beam according to a set path and movement parameters, and a polarization-dependent periodic micro-nano structure 18 is induced and generated at the focusing position of the ultrafast laser beam.
The periodic micro-nano structure is a strip-shaped micro-nano structure which is located on a focusing plane and is distributed periodically. In the specific implementation, as shown in fig. 4, the array is a form in which a plurality of bar structures are periodically arranged, and the plurality of bar structures are on the same focal plane.
Step seven: and after the processing is finished, turning off the laser beam, turning on a microscope illuminator 13 in a microscope observation system, observing the appearance of a processing area through a CCD camera 17 of the microscope observation system, and rotating the two polaroids 14-15 to ensure that the polarization directions of the two polaroids are mutually perpendicular to form a crossed polaroid. The image collected by the CCD camera shows that a polarization-dependent periodic micro-nano structure and a polarization-dependent periodic birefringence phenomenon appear, which indicates that a self-organized periodic micro-nano structure 18 is generated, and the specific morphology of the structure is shown in FIG. 4.
Example 2:
the method comprises the following steps: sample 11 was prepared by the suspension method, sample 11 being 35La ternary glass2O3-xTiO2-(65-x)Nb2O5(30 < x < 60), where x represents the mole percentage (mol.%).
By setting to adjust Ta2O5Or TiO2The larger x is, the stronger the crystallization ability of the sample 11 is, the easier the micro-nano structure is induced to be generated, and the faster the processing speed is used, but the more difficult the preparation of the sample 11 becomes. Ta of an embodiment of the invention2O5Or TiO2The preparation of the periodic micro-nano structure with the glass-crystal alternate arrangement can be well realized by the molar percentage x.
Step two: fixing the sample 11 on a displacement platform 12, finding a position suitable for processing through a microscopic observation system, and determining the xyz three-axis coordinates of the sample for setting motion parameters subsequently.
Step three: the machining path is imported into the computer 1, and the motion parameters of the specific machining path are as follows: setting the processing speed of 1000-;
step four: the processing laser parameters are led into the computer 1, and the specific laser parameters are as follows: setting the average power as a larger initial value of 3000mW to ensure the stability of laser output, the pulse width of 1-4ps and the repetition frequency of 100-200 kHz;
step five: the ultrafast laser 2 is started to make the ultrafast laser beam 19 enter the optical path system along the symmetrical central line, the passing and blocking of the ultrafast laser beam 19 are controlled by the shutter 3 in the optical path system, the polarization direction of the ultrafast laser beam 19 is controlled by the Glan Taylor prism 4 and the half-wave plate 5 in the optical path system, and the average power actually processed by the ultrafast laser beam 19 is adjusted to 150-300mW by the optical attenuator 6 in the optical path system. The ultrafast laser beam 19 passes through the mirrors 7 to 8 in the optical path system, and the dichroic mirror 9, enters the objective lens 10, and is focused inside the sample 11 through the objective lens 10.
Step six: and (3) statically irradiating the sample 11 by using a laser beam for a period of time, starting the displacement platform 12 when the sample 11 is excited by the ultrafast laser beam 19 to generate visible light, enabling the sample 11 to move relative to the laser beam according to a set path and a set motion parameter, and inducing the focus of the ultrafast laser beam to generate a polarization-dependent periodic micro-nano structure 18.
The periodic micro-nano structure is a strip-shaped micro-nano structure which is located on a focusing plane and is distributed periodically. In the specific implementation, as shown in fig. 4, the array is a form in which a plurality of bar structures are periodically arranged, and the plurality of bar structures are on the same focal plane.
Step seven: and after the processing is finished, turning off the laser beam, turning on a microscope illuminator 13 in a microscope observation system, observing the appearance of a processing area through a CCD camera 17 of the microscope observation system, and rotating the two polaroids 14-15 to ensure that the polarization directions of the two polaroids are mutually perpendicular to form a crossed polaroid. The image collected by the CCD camera shows that a polarization-dependent periodic micro-nano structure and a polarization-dependent periodic birefringence phenomenon appear, which indicates that a self-organized periodic micro-nano structure 18 is generated, and the specific morphology of the structure is shown in FIG. 4.
Originally, due to the arrangement of the crossed polaroid, the visible light beam emitted by the micro illuminator 13 cannot penetrate through the crossed polaroid, and no image of the light beam is acquired at the CCD camera; however, according to the technical scheme of the invention, the self-organized periodic micro-nano structure 18 grown on the inner surface of the glass can act on the visible light beam to deflect the polarization angle of the visible light beam, so that the light signal transmitted from the ultrafast laser processing area can be collected at the CCD camera through the second polaroid, and whether the micro-nano structure is generated or not is judged according to the light signal.
According to the invention, inhomogeneous particles or defects in the glass interact with an incident light field to generate plasma waves, and the plasma waves interfere with subsequently input light waves to cause the periodic distribution of the intensity of the light field in a focusing region, so that the periodic distribution of the density of the excited plasma is caused, and the periodic distribution of the temperature field is finally caused.
For the material 11 to be processed, the periodic distribution of the temperature field will induce selective devitrification inside the glass, the devitrified areas coinciding with the light field interference pattern and being periodic as well.
Because the crystallization only occurs in the nonlinear ionization region at the center of the focusing spot, the optical diffraction limit can be broken through, so that the selective crystallization has a nanoscale dimension, the direction of the selective crystallization depends on the polarization direction of incident laser, and a polarization-dependent micro-nano structure formed by alternately arranging glass and crystals can be formed under the condition of determining process parameters.
As shown in fig. 5, the periodic micro-nano structure obtained by the present invention can be used for manufacturing a micro optical attenuator 21 in an infrared band. During manufacturing, a plurality of self-organizing periodic micro-nano structures 18 are scanned at 40 micrometers below the surface of a sample at intervals of 15-20 micrometers to form a grating array, laser emitted by a laser 20 is diffracted when passing through the scanning line array, wherein the power of a zero-order diffraction spot is changed alternately in intensity along with the change of the polarization direction of the laser, and the intensity is caused by selective reflection and absorption of the periodic micro-nano structures to light in a specific polarization direction, so that the attenuator 21 can perform the light attenuation function with a small size.
Comparative example:
when La2O3-Nb2O5Ta in glass system2O5And TiO2When the content of the crystal is too low or not high, the crystallization capacity of the glass is greatly reduced, only the refractive index change of a local area can be generated under the action of ultrafast laser, and the periodic crystallization cannot be induced to form a regular crystal-glass alternate periodic micro-nano structure, so that the attenuation effect on optical signals cannot be generated. When La2O3-Nb2O5Ta in glass system2O5And TiO2When the content of (A) is too high, the crystallization capacity of a ternary system is too strong, the ternary system becomes ceramic after suspension smelting, and the ceramic cannot be made into glass and loses transparency, so that a micro-nano structure cannot be processed inside.
The current mature commercial attenuator adopts the coating film reflection principle to attenuate light, and the attenuator needs larger size to ensure the continuous and uniform change of the coating film thickness and is difficult to miniaturize and integrate. Meanwhile, the coated attenuator cannot bear high energy input and is easy to damage when used for attenuating infrared high-power laser.
The invention can realize the preparation of the periodic micro-nano structure for infrared high-power laser attenuation, realizes the high-efficiency preparation of the polarization-dependent periodic micro-nano structure, and expands functional materials for forming the periodic micro-nano structure.
Claims (9)
1. A preparation method of a self-organized periodic micro-nano structure with alternately arranged glass and crystals is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing a sample (11) by using a suspension method, wherein the sample (11) is ternary glass 35La2O3-xTa2O5-(65-x)Nb2O5(5 < x < 45) or 35La2O3-xTiO2-(65-x)Nb2O5(30 < x < 60), wherein x represents the mole percentage (mol.%);
s2: fixing a sample (11) on a displacement platform (12), wherein an ultrafast laser beam is emitted by an ultrafast laser (2), and is irradiated onto the sample (11) through a shutter (3), a Glan Taylor prism (4) and a half-wave plate (5) and focused into the sample (11);
s3: and (2) statically irradiating the sample (11) by using a laser beam for a period of time, starting a displacement platform (12) when the sample (11) at the focusing position is excited by the ultrafast laser beam to generate visible light, enabling the sample (11) to move relative to the laser beam according to a set path and movement parameters, and inducing the polarization-dependent periodic micro-nano structure at the focusing position of the laser beam.
2. The method for preparing the self-organized periodic micro-nano structure with alternately arranged glass and crystals according to claim 1, which is characterized in that: the passing and blocking of the laser light are controlled by a shutter (3) in the optical path system, the polarization direction of the laser beam is controlled by a Glan Taylor prism (4) and a half-wave plate (5) in the optical path system, and the average power of the laser beam is adjusted to 150-300mW by an optical attenuator (6) in the optical path system.
3. The method for preparing the self-organized periodic micro-nano structure with alternately arranged glass and crystals according to claim 1, which is characterized in that: the displacement platform (12) drives the sample (11) to do plane scanning movement, so that the laser beam does plane scanning movement relative to the laser beam at the focusing position inside the sample (11).
4. The method for preparing the self-organized periodic micro-nano structure with alternately arranged glass and crystals according to claim 1, which is characterized in that: the displacement platform (12) drives the sample (11) to do different motions to generate periodic micro-nano structures with different patterns.
5. The method for preparing the self-organized periodic micro-nano structure with alternately arranged glass and crystals according to claim 1, which is characterized in that: an ultrafast laser micro-nano processing and manufacturing system is adopted, and comprises a computer (1), an ultrafast laser (2), a shutter (3), a Glan Taylor prism (4), a half-wave plate (5), an optical attenuator (6), a first total reflector (7), a second total reflector (8), a dichroic mirror (9), an objective lens (10), a sample (11), a displacement platform (12), a micro illuminator (13), a first polarizing film (14), a second polarizing film (15), an eyepiece (16) and a CCD camera (17); an output ultrafast laser beam of the ultrafast laser (2) sequentially passes through a shutter (3), a Glan Taylor prism (4), a half-wave plate (5) and an optical attenuator (6), then enters a first total reflecting mirror (7), sequentially reflects through the first total reflecting mirror (7), a second total reflecting mirror (8) and a dichroic mirror (9), then irradiates a sample (11) through an objective lens (10) and focuses inside the sample (11); the sample (11) is fixedly arranged on a displacement platform (12), the microscopic illuminator (13) is positioned below the sample (11), the microscopic illuminator (13) emits a visible light beam upwards, the visible light beam enters the sample (11) through a first polaroid (14), the visible light beam penetrating through the sample (11) and the visible light excited by the ultrafast laser beam irradiating on the sample (11) are transmitted through a dichroic mirror (9), and then sequentially pass through a second polaroid (15) and an eyepiece (16) and enter a CCD camera (17) to be detected and received; and simultaneously, the computer (1) is respectively connected with the control ports of the ultrafast laser (2), the shutter (3), the displacement platform (12) and the CCD camera (17).
6. The method for preparing the self-organized periodic micro-nano structure with alternately arranged glass and crystals according to claim 1, which is characterized in that: the sample (11) is fixed on the displacement platform (12) through a clamp.
7. The method for preparing the self-organized periodic micro-nano structure with alternately arranged glass and crystals according to claim 5, which is characterized in that: the polarization directions of the first polarizer (14) and the second polarizer (15) are perpendicular, and the first polarizer (14) and the second polarizer (15) form a crossed polarizer.
8. A self-organized periodic micro-nano structure with alternately arranged glass and crystals is characterized in that: prepared by the process of any one of claims 1 to 7.
9. The use of the self-organized periodic micro-nano structure with glass and crystals alternately arranged according to claim 8, characterized in that: the self-organized periodic micro-nano structure is applied to the preparation of infrared optical attenuators.
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