CN114101901B - Processing technology capable of integrating micro-nano optical structure - Google Patents
Processing technology capable of integrating micro-nano optical structure Download PDFInfo
- Publication number
- CN114101901B CN114101901B CN202111476346.5A CN202111476346A CN114101901B CN 114101901 B CN114101901 B CN 114101901B CN 202111476346 A CN202111476346 A CN 202111476346A CN 114101901 B CN114101901 B CN 114101901B
- Authority
- CN
- China
- Prior art keywords
- crystal
- femtosecond laser
- micro
- nano
- titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 230000003287 optical effect Effects 0.000 title claims abstract description 50
- 238000012545 processing Methods 0.000 title claims abstract description 32
- 238000005516 engineering process Methods 0.000 title claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 84
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 25
- 239000010936 titanium Substances 0.000 claims abstract description 25
- 239000010437 gem Substances 0.000 claims abstract description 24
- 229910001751 gemstone Inorganic materials 0.000 claims abstract description 24
- 239000006184 cosolvent Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 230000010287 polarization Effects 0.000 claims abstract description 9
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000008569 process Effects 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims 1
- 239000010980 sapphire Substances 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000007716 flux method Methods 0.000 description 1
- 238000002017 high-resolution X-ray diffraction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- 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
- B23K26/062—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam
- B23K26/0622—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses
- B23K26/0624—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses using ultrashort pulses, i.e. pulses of 1ns or less
-
- 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
- B23K26/0093—Working by laser beam, e.g. welding, cutting or boring combined with mechanical machining or metal-working covered by other subclasses than B23K
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Laser Beam Processing (AREA)
- Lasers (AREA)
Abstract
A processing technology of an integrable micro-nano optical structure comprises the following steps: (1) growth: bi is mixed with 2 O 3 、TeO 2 、H 3 BO 3 Fully grinding and mixing, transferring to a muffle furnace, performing primary sintering for 10-12h, and cooling to obtain a primary sintering raw material; transferring the primary sintering raw material to a single crystal growth furnace for growth to obtain crystals; (2) polishing; (3) femtosecond laser: performing femtosecond laser micro-nano processing on the crystal by adopting a titanium precious stone femtosecond laser; the pulse width of the titanium gemstone femtosecond laser is set to be 100-120 fs of linear polarization laser, the center wavelength is set to 790-800nm, and the repetition frequency is set to be l-3kHz. The processing technology of the integrated micro-nano optical structure has reasonable design and adopts Te 2 O 3 ‑B 2 O 3 As a cosolvent, for Bi 2 O 3 、TeO 2 、H 3 BO 3 Bi is synthesized by adopting a fluxing agent method 3 TeBO 9 The crystal adopts the titanium precious stone femtosecond laser to carry out femtosecond laser micro-nano processing on the crystal, has high precision, three dimensions, small thermal effect and no pollution, forms an optical waveguide microstructure, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of optical structures, and particularly relates to a processing technology capable of integrating a micro-nano optical structure.
Background
Micro-nano optics is an important development direction of the novel photoelectron industry at present, and plays a great role in various fields such as optical communication, optical interconnection, optical storage, semiconductor devices and the like. The micro-nano optical structure technology refers to that a novel optical function device is manufactured by introducing a micro-nano optical structure into related materials. Micro-nano optics is the optical branch that utilizes microstructured materials as optical elements. The design and manufacture of the structure of the micro-nano optical system are key problems in the development of micro-nano optical technology, so that micro-nano optical system becomes a key breakthrough in the development of novel photoelectronic industry. Its main advantage is that it can realize many new functions based on local electromagnetic interaction, becoming an indispensable key science and technology in 21 st century.
The integrated optical circuit can realize high-speed, stable and low-loss transmission and processing of the optical signals in an integrated space. Through on-chip integration of various optical elements with different functions, an all-optical device with small volume, multiple functions, high speed and large capacity can be prepared on a substrate material, so that the method is widely applied to the fields of optical fiber communication, chemical sensing, biomedical treatment, environmental monitoring, spectral research, material science, photon computer research and the like. In order to better realize the integration of high-performance optical systems, a processing technology capable of integrating micro-nano optical structures needs to be developed.
Disclosure of Invention
The invention aims to: in order to overcome the defects, the invention aims to provide a processing technology capable of integrating a micro-nano optical structure, which has reasonable design and adopts Te 2 O 3 -B 2 O 3 As a cosolvent, for Bi 2 O 3 、TeO 2 、H 3 BO 3 Bi is synthesized by adopting a fluxing agent method 3 TeBO 9 The crystal adopts the titanium precious stone femtosecond laser to carry out femtosecond laser micro-nano processing on the crystal, has high precision, three dimensions, small thermal effect and no pollution, forms an optical waveguide microstructure, and has wide application prospect.
The invention aims at realizing the following technical scheme:
a processing technology of an integrable micro-nano optical structure comprises the following steps:
(1) And (3) growing: bi is mixed with 2 O 3 、TeO 2 、H 3 BO 3 Fully grinding and mixing, transferring to a muffle furnace, performing primary sintering for 10-12h, and cooling to obtain a primary sintering raw material; transferring the primary sintering raw material to a single crystal growth furnace, heating to 900-1000 ℃ at 50-100 ℃/h to obtain high Wen Rongye, keeping the temperature for 36-48 hours, and cooling to 10-20 ℃ above the saturation temperature at 10-30 ℃/h; fixing the lower end of the catalyst with a cosolvent Te 2 O 3 -B 2 O 3 The seed rod of the seed crystal stretches into the single crystal growth furnace from a small hole at the top of the single crystal growth furnace at a vertical pulling speed of 0.005-0.01mm/h, so that Te is obtained 2 O 3 -B 2 O 3 The seed crystal is contacted with the high-temperature melt or stretches into the high Wen Rongye; rotating Te at a rate of 20-30 rpm 2 O 3 -B 2 O 3 Seed crystal is kept constant for 0.5 to 1 hour at 5-cooling to saturation temperature at a cooling rate of 10 ℃/h; then cooling the grown crystal at a cooling rate of 0.1-0.3 ℃/day, and after growing for 120-150 days, lifting the crystal to separate from the liquid level to obtain the crystal;
(2) Polishing: cutting the crystal into a size of a multiplied by b multiplied by c, wherein a is 1-3mm, b is 8-10 mm, c is 8-10 mm, and performing optical polishing treatment on the crystal;
(3) Femtosecond laser: performing femtosecond laser micro-nano processing on the crystal by adopting a titanium precious stone femtosecond laser; the pulse width of the titanium gemstone femtosecond laser is set to be 100-120 fs of linear polarization laser, the center wavelength is set to 790-800nm, and the repetition frequency is set to be l-3kHz.
The processing technology of the integrated micro-nano optical structure has reasonable design and uses Bi 3 TeBO 9 As a cosolvent, for Bi 2 O 3 、TeO 2 、H 3 BO 3 Bi is synthesized by adopting a fluxing agent method 3 Te BO 9 The crystal overcomes the problems of melt layering and higher viscosity, and obtains Bi with centimeter size 3 TeBO 9 The crystal quality of the grown crystal is good. The Bi is 3 Te BO 9 The crystal has a maximum SHG coefficient of about 20 times that of the KDP crystal. Wherein Te is 2 O 3 - B 2 O 3 The seed rod of the seed crystal stretches into the single crystal growth furnace from a small hole at the top of the single crystal growth furnace at a vertical pulling speed of 0.005-0.01mm/h, and a vertical pulling process is arranged and a lower pulling speed is used to ensure that a growth interface is always maintained near the surface of the boron-rich melt, so that melt layering caused by the density difference of raw materials is reduced; to overcome the problem of higher melt viscosity and minimize melt delamination, bi is spun at a rate of 20-30 rpm 3 TeBO 9 And (5) seed crystal.
The invention adopts the titanium precious stone femtosecond laser to carry out femtosecond laser micro-nano processing on the crystal, and focused femtosecond pulse laser constructs a three-dimensional micro-nano structure in the crystal according to a design pattern, and has the advantages of high precision, three-dimension, small thermal effect, no pollution and the like. The refractive index of the processing region is changed through the interaction of the laser and the crystalline dielectric material, so that the optical waveguide microstructure is formed.
Further, in the processing technology of the integrable micro-nano optical structure, the growth process in the step (1) requires participation of oxygen, and the Bi is configured 2 O 3 、TeO 2 、H 3 BO 3 The molar ratio of (2) is 3:2:2.
The reaction equation is as follows: 3Bi 2 O 3 ＋2TeO 2 ＋2H 3 BO 3 ＋O 2 →2 Bi 3 TeBO 9 ＋３H 2 O 。 Further, in the processing technology of the integrable micro-nano optical structure, in the step (1), the cosolvent Te 2 O 3 - B 2 O 3 The mass ratio of the cosolvent Te to the crystal is 1:3-5, and the cosolvent Te is prepared from the cosolvent Te 2 O 3 -B 2 O 3 Middle Te 2 O 3 And B is connected with 2 O 3 The molar ratio of (2) is 3:1.
The invention adopts Te 2 O 3 - B 2 O 3 As a cosolvent, according to Te 2 O 3 - B 2 O 3 Phase diagram ， Te 2 O 3 And B is connected with 2 O 3 Has a minimum melting point of B 2 O 3 =25.5 mol%, when Te 2 O 3 And B is connected with 2 O 3 Te in a molar ratio of 3:1 2 O 3 - B 2 O 3 The melting temperature of the system is lower, and the fluxing agent system can effectively reduce the melting temperature of the raw materials at about 680 ℃.
Further, in the processing technology of the integrable micro-nano optical structure, in the step (1), the temperature of preliminary sintering is set to be 500-550 ℃; the saturation temperature was 795 ℃.
In the step (2), before the micro-nano processing of the femtosecond laser, a neutral density filter is adopted to perform coarse adjustment on the titanium gemstone femtosecond laser, and then a series of half wave plates and linear polarizers positioned in front of the neutral density filter are adopted to perform continuous fine adjustment until the monopulse energy of the titanium gemstone femtosecond laser acting on the crystal is 0.8-0.9 mu J.
Further, in the processing technology of the integrable micro-nano optical structure, in the step (2), the operation steps of the titanium gemstone femtosecond laser are as follows: the femtosecond laser beam of the titanium gemstone femtosecond laser is focused below the b x c surface of the crystal by a microscope objective lens with a numerical aperture of 0.4 and a magnification of 20x, the crystal positioned on a three-dimensional electric platform is scanned and processed along the b axis direction at a speed of 0.1-0.3mm/s, and damage marks with the length of 5-8 mu m are formed on the a x b end surface and the a x c end surface of the crystal.
Further, the processing technology of the integrable micro-nano optical structure repeats the operation steps, and performs parallel scanning for several times at different positions of the crystal until a periodic array structure with a hexagonal cross section is formed, and the transverse interval between two adjacent damage traces is 5-8 μm.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention relates to a processing technology of an integrable micro-nano optical structure, which uses Te 2 O 3 -B 2 O 3 As a cosolvent, for Bi 2 O 3 、TeO 2 、H 3 BO 3 Bi is synthesized by adopting a fluxing agent method 3 TeBO 9 The crystal overcomes the problems of melt layering and higher viscosity, and obtains Bi with centimeter size 3 TeBO 9 The crystal quality of the grown crystal is good;
(2) According to the processing technology of the integrated micro-nano optical structure, the titanium precious stone femtosecond laser is adopted to carry out femtosecond laser micro-nano processing on the crystal, and the focused femtosecond pulse laser builds a three-dimensional micro-nano structure in the crystal according to the design pattern, so that the processing technology has the advantages of high precision, three dimensions, small thermal effect, no pollution and the like. The refractive index of the processing region is changed through the interaction of the laser and the crystalline dielectric material, so that the optical waveguide microstructure is formed.
Drawings
FIG. 1 is a graph showing the rocking curves of the (200) and (002) planes of a crystal obtained in example 1 of an integrable micro-nano optical structure according to the present invention;
fig. 2 is a graph showing the change of the transmission power of the micro-nano optical structure obtained in the embodiment 2 of the present invention with the same 1064-nm full-angle incident light power;
Detailed Description
The following examples are given in conjunction with fig. 1-2 and detailed experimental data to clearly and completely describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The following examples provide a process for the fabrication of an integrable micro-nano optical structure.
Example 1
Preparation of crystals
Bi is mixed with 2 O 3 、TeO 2 、H 3 BO 3 Fully grinding and mixing the Bi 2 O 3 、TeO 2 、H 3 BO 3 The molar ratio of (2) is 3:2:2, then the mixture is transferred into a muffle furnace for preliminary sintering for 12 hours, the preliminary sintering temperature is set to 520 ℃, and after cooling, the primary sintering raw material is obtained; transferring the primary sintering raw material to a single crystal growth furnace, heating to 1000 ℃ at 60 ℃/h to obtain high Wen Rongye, keeping the temperature for 36 hours, and cooling to 810 ℃ at 20 ℃/h; fixing the lower end of the catalyst with a cosolvent Te 2 O 3 -B 2 The seed rod of the O seed crystal stretches into the single crystal growth furnace from a small hole at the top of the single crystal growth furnace at a vertical pulling speed of 0.005mm/h, so that Te is obtained 2 O 3 -B 2 The O seed crystal and the high-temperature melt extend into the high Wen Rongye; te was rotated at 30 rpm 2 O 3 -B 2 O 3 Seed crystal is kept at constant temperature for 1 hour, and the temperature is reduced to the saturation temperature of 795 ℃ at the temperature reduction rate of 5 ℃/h; then cooling the grown crystal at a cooling rate of 0.1 ℃/day, and after growing for 120-150 days, lifting the crystal to separate from the liquid surface to obtain the crystal of the example 1.
Example 2
The crystals obtained in example 1 were further subjected to the preparation of integrable micro-nano optical structures.
Cutting the crystal into a dimension of a multiplied by b multiplied by c, wherein a is 2mm, b is 10 mm, c is 100 mm, and performing optical polishing treatment on the crystal; femtosecond laser: performing femtosecond laser micro-nano processing on the crystal by adopting a titanium precious stone femtosecond laser; before micro-nano processing of the femtosecond laser, firstly adopting a neutral density filter to coarsely adjust the titanium gemstone femtosecond laser, and then adopting a series of half wave plates and linear polarizers positioned in front of the neutral density filter to continuously finely adjust the titanium gemstone femtosecond laser until the single pulse energy of the titanium gemstone femtosecond laser acting on the crystal is 0.8 mu J; the pulse width of the titanium gemstone femtosecond laser is set as 100 fs of linear polarization laser, the center wavelength is set as 795nm, and the repetition frequency is set as 2kHz.
The operation steps of the titanium precious stone femtosecond laser are as follows: the femtosecond laser beam of the titanium gemstone femtosecond laser is focused below the b x c surface of the above crystal by a microscope objective lens with a numerical aperture of 0.4 and a magnification of 20x, scanning processing is carried out on the above crystal positioned on a three-dimensional electric platform along the b axis direction at a speed of 0.1mm/s, damage marks with a length of 8 μm are formed on the a x b end surface and the a x c end surface of the above crystal, parallel scanning is carried out for a plurality of times at different positions of the above crystal until a periodic array structure with a hexagonal cross section is formed, and the transverse interval between two adjacent damage marks is 5-8 μm.
And (3) effect verification:
the crystal quality of the crystal obtained in example 1 and the crystal obtained in comparative example 1 described above were examined, and the rocking curves of the (200) and (002) planes were measured by a high-resolution XRD diffractometer, and the results are shown in fig. 1.
The test results showed that the rocking curves of the (200) and (002) planes of the crystals obtained in example 1 were excellent in symmetry, sharp in peak shape without cleavage, and half-width (FWHM) was 62.23 "and 53.12", respectively, which indicates Bi of example 1 grown by the flux method 3 TeBO 9 The crystallinity of the single crystal is higher.
The integrable micronano optical structure obtained by the above example 2 was subjected to a guided wave property detection, and the guided wave property detection transmission characteristic test was based on a typical end-face coupling system. The probe light is a linearly polarized laser light with a wavelength of 1064nm output by a continuous solid state laser. The polarization direction of the incident probe light is adjusted by the half-wave plate, and the polarization characteristics of the integrable micro-nano optical structure obtained in the above embodiment 2 in the light transmission are detected. The laser is converged and coupled to the incident end face of the waveguide through a microscope objective with the magnification of 25x, and is collected into a near-infrared CCD camera from the emergent end face of the waveguide microstructure through another objective with the same parameters, so that the near-field mode distribution of different light guide microstructures is displayed. The transmission loss of the microstructure can be obtained by directly detecting the power calculation of the incident and emergent ends of the transmission laser, and the result is shown in fig. 2.
The test results show that the laser power transmitted by the integrable micro-nano optical structure obtained in the embodiment 2 along each polarization direction is almost the same, so that the light guide transmission in all-angle directions can be supported, and the transmission performance is more excellent.
Furthermore, the integrable micronano-optical structures obtained in example 2 above have losses of 0.58dB and 0.50dB under TM and TE polarization, respectively, exhibiting excellent transmission of their microstructures in orthogonal polarization directions.
In summary, the integrable micro-nano optical structure obtained in the above embodiment 2 shows excellent waveguide performance, which lays a good foundation for integration of the multifunctional photonics device.
There are many ways in which the invention may be practiced, and what has been described above is merely a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that modifications may be made without departing from the principles of the invention, and such modifications are intended to be within the scope of the invention.
Claims (6)
1. The processing technology of the integrated micro-nano optical structure is characterized by comprising the following steps of:
(1) And (3) growing: bi is mixed with 2 O 3 、TeO 2 、H 3 BO 3 Fully grinding and mixing, transferring to a muffle furnace, performing primary sintering for 10-12h, and cooling to obtain a primary sintering raw material; transferring the primary sintering raw material to a single crystal growth furnace, heating to 900-1000 ℃ at 50-100 ℃/h to obtain high Wen Rongye, keeping the temperature for 36-48 hours, and cooling to 10-20 ℃ above the saturation temperature at 10-30 ℃/h; fixing the lower end of the catalyst with a cosolvent Te 2 O 3 -B 2 O 3 The seed rod of the seed crystal stretches into the single crystal growth furnace from a small hole at the top of the single crystal growth furnace at a vertical pulling speed of 0.005-0.01mm/h, so that Te is obtained 2 O 3 -B 2 O 3 The seed crystal is contacted with the high-temperature melt or stretches into the high Wen Rongye; rotating Te at a rate of 20-30 rpm 2 O 3 -B 2 O 3 Seed crystal is kept at constant temperature for 0.5-1 hour, and the temperature is reduced to saturation temperature at a temperature reduction rate of 5-10 ℃/h; then cooling the grown crystal at a cooling rate of 0.1-0.3 ℃/day, and after growing for 120-150 days, lifting the crystal to separate from the liquid level to obtain the crystal;
(2) Polishing: cutting the crystal into a size of a multiplied by b multiplied by c, wherein a is 1-3mm, b is 8-10 mm, c is 8-10 mm, and performing optical polishing treatment on the crystal;
(3): firstly, coarse adjustment is carried out on a titanium precious stone femtosecond laser by adopting a neutral density filter, then a series of half wave plates and linear polarizers positioned in front of the neutral density filter are adopted for continuous fine adjustment until the single pulse energy of the titanium precious stone femtosecond laser acting on the crystal is 0.8-0.9 mu J, and then the titanium precious stone femtosecond laser is adopted for carrying out femtosecond laser micro-nano processing on the crystal; the pulse width of the titanium gemstone femtosecond laser is set to be 100-120 fs of linear polarization laser, the center wavelength is set to 790-800nm, and the repetition frequency is set to be l-3kHz.
2. The process of claim 1, wherein the growth in step (1) requires oxygen and is configured as Bi 2 O 3 、TeO 2 、H 3 BO 3 Molar of (2)The ratio is 3:2:2.
3. The process of claim 1, wherein in step (1), the cosolvent Te 2 O 3 - B 2 O 3 The mass ratio of the cosolvent Te to the crystal is 1:3-5, and the cosolvent Te is prepared from the cosolvent Te 2 O 3 -B 2 O 3 Middle Te 2 O 3 And B is connected with 2 O 3 The molar ratio of (2) is 3:1.
4. The process for fabricating an integrable micro-nano optical structure according to claim 1, wherein in step (1), the temperature of preliminary sintering is set to 500-550 ℃; the saturation temperature was 795 ℃.
5. The process for fabricating an integrable micro-nano optical structure according to claim 1, wherein in the step (2), the operation steps of the titanium sapphire femtosecond laser are as follows: the femtosecond laser beam of the titanium gemstone femtosecond laser is focused below the b x c surface of the crystal by a microscope objective lens with a numerical aperture of 0.4 and a magnification of 20x, the crystal positioned on a three-dimensional electric platform is scanned and processed along the b axis direction at a speed of 0.1-0.3mm/s, and damage marks with the length of 5-8 mu m are formed on the a x b end surface and the a x c end surface of the crystal.
6. The process of claim 5, wherein the steps are repeated, and the crystal is scanned in parallel at different positions until a periodic array structure with hexagonal cross section is formed, and the lateral spacing between two adjacent damage tracks is 5-8 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111476346.5A CN114101901B (en) | 2021-12-06 | 2021-12-06 | Processing technology capable of integrating micro-nano optical structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111476346.5A CN114101901B (en) | 2021-12-06 | 2021-12-06 | Processing technology capable of integrating micro-nano optical structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114101901A CN114101901A (en) | 2022-03-01 |
| CN114101901B true CN114101901B (en) | 2024-01-05 |
Family
ID=80367091
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111476346.5A Active CN114101901B (en) | 2021-12-06 | 2021-12-06 | Processing technology capable of integrating micro-nano optical structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114101901B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914809A (en) * | 2010-08-11 | 2010-12-15 | 中国科学院新疆理化技术研究所 | Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof |
| CN102337591A (en) * | 2011-11-14 | 2012-02-01 | 西北大学 | Ytterbium-doped potassium triyttrium borate laser crystal, and growing method and application thereof |
| CN105128157A (en) * | 2015-06-18 | 2015-12-09 | 江苏苏创光学器材有限公司 | Manufacturing method for sapphire fingerprint recognition panel |
| CN105171941A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Preparing method for sapphire touch screen panel |
| CN105350083A (en) * | 2015-11-20 | 2016-02-24 | 中国科学院理化技术研究所 | (Bi1-x-yLnxCey)3TeBO9 compound, (Bi1-x-yLnxCey)3TeBO9 nonlinear optical crystal, (Bi1-x-yLnxCey)3TeBO9 scintillation crystal, preparation method and application thereof |
| CN109596243A (en) * | 2018-11-06 | 2019-04-09 | 天津大学 | Sapphire fiber Fabry-Perot sensor and preparation method thereof based on femtosecond laser etching |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10670806B2 (en) * | 2018-05-08 | 2020-06-02 | Shanghai Institute Of Optics And Fine Mechanics, Chinese Academy Of Sciences | Method for preparing film micro-optical structure based on photolithography and chemomechanical polishing |
-
2021
- 2021-12-06 CN CN202111476346.5A patent/CN114101901B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914809A (en) * | 2010-08-11 | 2010-12-15 | 中国科学院新疆理化技术研究所 | Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof |
| CN102337591A (en) * | 2011-11-14 | 2012-02-01 | 西北大学 | Ytterbium-doped potassium triyttrium borate laser crystal, and growing method and application thereof |
| CN105128157A (en) * | 2015-06-18 | 2015-12-09 | 江苏苏创光学器材有限公司 | Manufacturing method for sapphire fingerprint recognition panel |
| CN105171941A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Preparing method for sapphire touch screen panel |
| CN105350083A (en) * | 2015-11-20 | 2016-02-24 | 中国科学院理化技术研究所 | (Bi1-x-yLnxCey)3TeBO9 compound, (Bi1-x-yLnxCey)3TeBO9 nonlinear optical crystal, (Bi1-x-yLnxCey)3TeBO9 scintillation crystal, preparation method and application thereof |
| CN109596243A (en) * | 2018-11-06 | 2019-04-09 | 天津大学 | Sapphire fiber Fabry-Perot sensor and preparation method thereof based on femtosecond laser etching |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114101901A (en) | 2022-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jia et al. | Ion-cut lithium niobate on insulator technology: Recent advances and perspectives | |
| Singh et al. | Bismuth oxide and bismuth oxide doped glasses for optical and photonic applications | |
| CN110568694B (en) | Frequency converter based on ridge-type lithium niobate single crystal thin film waveguide integrated periodic domain inversion structure and preparation method thereof | |
| CN109477985A (en) | Substrate with dielectric film and the optical modulation element using it | |
| Zhang et al. | Femtosecond laser modification of 6H–SiC crystals for waveguide devices | |
| Wang et al. | Single crystal fibers: diversified functional crystal material | |
| CN110133802A (en) | A kind of novel lithium niobate optical waveguide wafer and preparation method thereof | |
| Liu et al. | Silicon nitride waveguides with directly grown WS 2 for efficient second-harmonic generation | |
| Huang et al. | Large quadratic electro-optic effect of the plzt thin films for optical communication integrated devices | |
| CN114101901B (en) | Processing technology capable of integrating micro-nano optical structure | |
| US20120156119A1 (en) | Nonlinear optic glassy fibers, methods of making and applications of the same | |
| Chaliha et al. | Luminescence and dielectric properties of nano-structured Eu3+: K2O–Nb2O5–SiO2 glass-ceramics | |
| CN107632341B (en) | Preparation method of three-dimensional waveguide type beam splitter in double-doped CaF 2 crystal | |
| CN105093406A (en) | Lithium niobate optical waveguide and method for preparing near-stoichiometric lithium niobate optical waveguide by means of titanium diffusion and vapor transport equilibration (VTE) | |
| US20230203326A1 (en) | 3d printed silica with nanoscale resolution | |
| Martinez-Jimenez et al. | Photonic micro-structures produced by selective etching of laser-crystallized amorphous silicon | |
| Burek et al. | High-q optical nanocavities in bulk single-crystal diamond | |
| Poberaj et al. | High-density integrated optics in ion-sliced lithium niobate thin films | |
| de Oliveira et al. | Fabrication and characterization of silicon nitride waveguides for mid-infrared applications | |
| Bagheri et al. | Impact of Non-Vertical Sidewalls on Bandgap Characteristics of LiNbO 3 Photonic Crystals | |
| Balasubramanian et al. | Growth and characterization of single crystal cored fibers (SCCF) of novel nonlinear organic optical materials | |
| Chen et al. | 3D Laser Writing of Low‐Loss Cross‐Section‐Variable Type‐I Optical Waveguide Passive/Active Integrated Devices in Single Crystals | |
| Gottlieb et al. | Noncollinear acousto-optic tunable filter: thallium phosphorus selenide system | |
| Chen et al. | Boosted Second Harmonic Generation and Cascaded Sum Frequency Generation from a Surface Crystallized Glass Ceramic Microcavity | |
| Xu et al. | Direct writing waveguides inside YAG crystal by femtosecond laser |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |