CN115536251A - High-precision molded sulfur optical device with super-structure surface structure and preparation method thereof - Google Patents

High-precision molded sulfur optical device with super-structure surface structure and preparation method thereof Download PDF

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Publication number
CN115536251A
CN115536251A CN202211317785.6A CN202211317785A CN115536251A CN 115536251 A CN115536251 A CN 115536251A CN 202211317785 A CN202211317785 A CN 202211317785A CN 115536251 A CN115536251 A CN 115536251A
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temperature
super
chalcogenide
glass
sulfur
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张鸣杰
陈媛芝
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Jinan University
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Jinan University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00Re-forming shaped glass
    • C03B23/02Re-forming glass sheets
    • C03B23/023Re-forming glass sheets by bending
    • C03B23/03Re-forming glass sheets by bending by press-bending between shaping moulds
    • C03B23/0305Press-bending accelerated by applying mechanical forces, e.g. inertia, weights or local forces
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00Re-forming shaped glass
    • C03B23/0013Re-forming shaped glass by pressing
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/002Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a high-precision molded sulfur optical device with a super-structure surface structure and a preparation method thereof, wherein the method comprises the following steps: transferring the designed super-structure surface structure pattern to a mould pressing mould core; pretreating a chalcogenide preform; putting the pretreated chalcogenide preform into the center of a lower mold core of a precision mold pressing die, sleeving the lower mold core into a mold sleeve, and putting an upper mold core into the mold sleeve; placing the precision mould pressing mould into mould pressing equipment, and slowly heating; performing mould pressing operation when the temperature is raised to a preset temperature above the glass transition temperature of the chalcogenide glass, and transferring the super-surface structure pattern on the mould core to the surface of the chalcogenide glass; keeping the pressure and the temperature for a preset time; slowly reducing the pressure and cooling; stopping pressing when the temperature is lower than the glass transition temperature of the chalcogenide glass; slowly cooling to the discharge temperature to obtain the chalcogenide glass optical component with the super-structure surface.

Description

High-precision molded sulfur optical device with super-structure surface structure and preparation method thereof
Technical Field
The invention belongs to the field of forming and processing of nano photonic components, and particularly relates to a high-precision die pressing preparation method of a chalcogenide glass-based optical component with an ultra-structure surface, in particular to a chalcogenide optical component with an ultra-structure surface structure and a preparation method thereof.
Background
With the rapid development of information technologies such as artificial intelligence, 5G communication, and high-end chips, the transmission, processing, and storage technologies of large capacity and large bandwidth of optical information become inevitable trends, leading to urgent needs for high-performance and high-integration optical information technologies and light-weight, miniaturized, and integrated nano optical components, and promoting the continuous development of optical field regulation and control technologies under micro-nano scale.
Metamorphic surfaces (metassurfaces) are two-dimensional metamaterials formed by sub-wavelength scale planar artificial atoms arranged in a particular structural manner. The artificial atoms can be regarded as local micro-nano optical antennas, and random regulation and control of local characteristics such as polarization, phase, amplitude and the like of light waves can be realized through careful design, so that novel physical phenomena and micro-nano optical devices are constructed. The metamaterial surface has the advantages of high integration level, planarization, low loss and the like, so that the requirements of people on miniaturization, high integration and multifunctional optical devices in the future are greatly met, and the metamaterial can be applied to multiple fields such as a modulation mechanism from corner optics to continuum bound state, a single-phase and multi-dimensional multi-parameter to topological state, a holographic image and a metamaterial lens to image processing application and the like. However, at present, the preparation of the optical component with the super-structure surface needs to adopt a micro-nano processing technology compatible with the CMOS, so that the preparation technology is complex, the structure with high depth-to-width ratio is difficult to complete, the yield is not high, and the cost is high.
The chalcogenide glass is an oxygen-free infrared glass material (the spectrum transmission range is from visible to 25 mu m) formed by three elements of S (sulfur), se (selenium) and Te (tellurium) of VIA group in the periodic table of elements and other metal elements such As Ge (germanium), ga (gallium), as (arsenic), sb (antimony), and the like, has the characteristics of low thermal temperature coefficient, easy preparation, low cost and the like compared with crystal materials such As germanium, selenium sulfide, zinc selenide and the like, and can be widely applied to infrared systems such As night vision gun aiming, automobile night vision, security monitoring, infrared temperature measurement and the like. Because the glass transition temperature of the chalcogenide glass is moderate (Tg-150-400 ℃), high-precision optical components with high precision and complex molded surfaces can be produced in batches by adopting a die pressing technology.
The invention combines the advantages of the optical element with the ultra-structure surface and the chalcogenide glass, processes the chalcogenide optical element with the ultra-structure surface by adopting the mould pressing technology, can further develop the chalcogenide optical element with special function, realizes the development of the optical element towards the directions of low cost, small size and light weight, and lays a foundation for developing the development and application of the chalcogenide glass in multiple fields.
Disclosure of Invention
To overcome the above-mentioned deficiencies of the prior art, the present invention provides a high-precision molded optical device with a super-structured surface structure and a method for manufacturing the same, which solves at least one of the above-mentioned problems.
According to one aspect of the present disclosure, there is provided a method for manufacturing a high-precision molded chalcogenide optical device with a super-structure surface structure, comprising the steps of:
firstly, transferring a designed super-structure surface structure pattern to a mould pressing mould core;
step two, pretreating a sulfur system preform;
thirdly, placing the pretreated chalcogenide preform into the center of a lower mold core of a precise mold pressing mold, sleeving the lower mold core into a mold sleeve, and then placing an upper mold core into the mold sleeve;
putting the precision mould pressing die into mould pressing equipment, and slowly heating;
step five, performing mould pressing operation when the temperature rises to a preset temperature above the glass transition temperature of the chalcogenide glass, and transferring the super-surface structure pattern on the mould core to the surface of the chalcogenide glass;
step six, keeping the pressure and the temperature for a preset time;
step seven, slowly reducing the pressure and cooling;
step eight, stopping applying the pressure when the temperature is lower than the glass transition temperature of the chalcogenide glass;
and step nine, slowly cooling to the discharging temperature to obtain the chalcogenide glass optical component with the super-structure surface.
The technical scheme combines the advantages of the super-structured surface in the aspect of optical component design and the characteristic that the chalcogenide glass is convenient for large-scale batch die pressing production, and provides a forming processing method of the optical component based on the chalcogenide glass super-structured surface structure so as to prepare the die pressing chalcogenide optical component with the super-structured surface structure.
Furthermore, the technical scheme is matched with a high-precision high-purity atmosphere control technology, the patterns of the super-structure surface structure and the surface shape of the die can be accurately transferred to chalcogenide glass, and the chalcogenide glass optical component with the super-structure surface structure is smoothly prepared.
Preferably, the designed pattern of the superstructure is single-sided or double-sided.
Specifically, the designed super-surface structure pattern can be only single-sided and can be transferred to an upper mold core or a lower mold core; it may also be double-sided and transferred onto the upper and lower cores simultaneously.
Preferably, a sheet-shaped or spherical sulfur-based preform is used as the sulfur-based preform.
Specifically, a sheet preform may be used if the molded component has a planar super-surface structure, and a spherical preform may be used if the molded component has a spherical or aspherical super-surface structure.
Preferably, the rate of temperature rise of the molding device is not greater than 10 ℃/s and the rate of temperature drop of the molding device is not greater than 10 ℃/s.
Preferably, the temperature at which the pressure application is started is not less than 5 ℃ above the glass transition temperature of the chalcogenide glass, and the temperature at which the pressure application is stopped is not more than 5 ℃ below the glass transition temperature of the chalcogenide glass.
Preferably, the pressure of the molding is not more than 10000N.
Preferably, the duration of holding the pressure and temperature is not less than 5s.
Preferably, the discharge temperature is not greater than 100 ℃.
Preferably, the method further comprises: and annealing the chalcogenide glass optical component with the super-structured surface at the annealing temperature of not less than 50 ℃ for not less than 10min.
According to one aspect of the present specification, there is also provided a high-precision molded, super-structured surface-structured chalcogenide optical device prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
(1) Compared with the existing super-structure surface structure device, the invention adopts a simple mould pressing technology to replace micro-nano etching technologies such as focused ion beam etching (FIB) and Electron Beam Lithography (EBL), can realize mass forming preparation, can simplify the preparation flow and greatly reduce the preparation cost.
(2) Compared with the traditional molded chalcogenide glass and other lenses, the invention adds the super-structure surface structure on the basis of the traditional molding technology, can further flexibly realize the manufacture of various optical components in multiple dimensions, and can realize the miniaturization, the light weight and the like of devices.
Drawings
Fig. 1 is a flow chart of a manufacturing method according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of a high-precision molded, super-textured surface structured chalcogenide optical device according to an embodiment of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be described below clearly and completely with reference to the accompanying drawings, and it is to be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
The invention provides a preparation method of a high-precision molded sulfur optical device with a super-structure surface structure, which comprises the following steps as shown in figure 1:
firstly, transferring a designed super-structure surface structure pattern to a mould pressing mould core;
step two, pretreating a chalcogenide preform;
thirdly, placing the pretreated chalcogenide preform into the center of a lower mold core of a precision mold pressing die, sleeving the lower mold core into a mold sleeve, and then placing an upper mold core into the mold sleeve;
putting the precision mould pressing die into mould pressing equipment, and slowly heating;
fifthly, the temperature is raised to a proper temperature above the glass transition temperature of the chalcogenide glass, the mould pressing operation is carried out, and the super-surface structure pattern on the mould core is transferred to the surface of the chalcogenide glass;
step six, keeping the pressure and the temperature;
step seven, slowly reducing the pressure and cooling;
step eight, stopping applying the pressure when the temperature is lower than the glass transition temperature of the chalcogenide glass;
step nine, slowly cooling to the discharging temperature to obtain the chalcogenide glass optical component with the super-structure surface;
step ten, annealing the chalcogenide glass optical component with the super-structure surface.
The high-precision molded sulfur-based optical device with the double-plane super-structure surface structure prepared by the method is shown in FIG. 2.
The present invention will now be described in detail and specifically with reference to the following examples so as to provide a better understanding of the present invention, but the following examples are not intended to limit the scope of the present invention.
Example one
This example illustrates the practice of the present invention in the context of processing a planar chalcogenide glass lens having a superstructural surface, using a chalcogenide material As a commercial chalcogenide glass 2 Se 3 (IG6):
1. Designing a super-structure surface structure with a focusing function according to parameters such as refractive index of IG6 glass, and transferring the super-structure surface structure onto an upper mold core of a mold pressing mold;
2. cutting and cleaning sheet-shaped IG6 glass as a preform;
3. putting the preform into the center of a lower mold core of a clean precision mold pressing die, sleeving the lower mold core on a mold sleeve, and putting the upper mold core into the mold sleeve;
4. placing the precision mould pressing die into mould pressing equipment, and heating to 250 ℃ at a speed of 1 ℃/min;
5. applying pressure to the mold at a rate of 1N/s to 350N;
6. maintaining the pressure and temperature for 10min;
7. reducing the pressure at 5N/min and reducing the temperature at 2 ℃/min;
8. stopping applying the pressure when the temperature is as low as 150 ℃;
9. cooling to 35 ℃ at a speed of 1 ℃/min, and taking out the planar chalcogenide glass lens with the super-structured surface;
10. the flat chalcogenide glass lens was annealed at 150 ℃ for 12 hours.
The plane IG6 glass lens with the super-structured surface prepared by the embodiment has good appearance and meets the requirements of finished lens products.
Example two
This example illustrates the implementation of the present invention by taking the processing of a planar chalcogenide glass beam deflector with a metamaterial surface as an example, and the chalcogenide material used is commercial chalcogenide glass Ge 28 Sb 12 Se 60 (IG5):
1. Designing a super-structure surface structure with a light beam deflection function according to parameters such as refractive index of IG5 glass, and transferring the super-structure surface structure onto an upper mold core of a mold pressing mold;
2. cutting and cleaning sheet-shaped IG5 glass as a preform;
3. putting the preform into the center of a lower mold core of a clean precision mold pressing die, sleeving the lower mold core on a mold sleeve, and putting the upper mold core into the mold sleeve;
4. placing the precision mould pressing mould into mould pressing equipment, and heating to 320 ℃ at the speed of 1 ℃/min;
5. applying pressure to the mold at a rate of 1N/s to 500N;
6. keeping the pressure and temperature for 15min;
7. reducing the pressure at 8N/min and reducing the temperature at 2 ℃/min;
8. stopping pressing when the temperature is low to 250 ℃;
9. cooling to 35 deg.C at 1 deg.C/min, and taking out the planar chalcogenide glass beam deflector with a super-structured surface;
10. annealing the planar chalcogenide glass beam deflector at 230 ℃ for 24h.
The plane IG5 glass beam deflection device with the super-structured surface is prepared by the embodiment, the device is good in appearance, and the requirements of finished products of the beam deflection device are met.
EXAMPLE III
This example specifically illustrates the implementation of the present invention by taking the example of processing a polarization converter of spherical chalcogenide glass with a super-structured surface, and the chalcogenide material used is commercial chalcogenide glass Ge 10 As 40 Se 50 (IG4):
1. Designing a super-structure surface structure with a broadband polarization conversion function according to parameters such as refractive index of IG4 glass, and transferring the super-structure surface structure onto an upper mold core of a mold pressing mold;
2. cutting and cleaning spherical IG4 glass as a preform;
3. putting the preform into the center of a lower mold core of a clean precision mold pressing die, sleeving the lower mold core on a mold sleeve, and putting the upper mold core into the mold sleeve;
4. placing the precision mould pressing mould into mould pressing equipment, and heating to 240 ℃ at the speed of 1 ℃/min;
5. applying pressure to the mold at a rate of 1N/s to 300N;
6. keeping the pressure and temperature for 10min;
7. reducing the pressure by 10N/min and reducing the temperature by 2 ℃/min;
8. stopping pressing when the temperature is lowered to 200 ℃;
9. cooling to 35 ℃ at a speed of 1 ℃/min, and taking out the broadband polarization conversion device with the super-structured surface;
10. the spherical chalcogenide glass polarization converter was annealed at 200 ℃ for 15h.
The plane IG4 glass deflection conversion device with the super-structured surface is prepared by the embodiment, the appearance of the device is good, and the requirements of finished products of the light beam conversion device are met.
Example four
This example illustrates the implementation of the present invention by taking the example of processing an aspheric chalcogenide glass vortex light generator with a super-structured surface, and the chalcogenide material used is commercial chalcogenide glass Ge 33 As 12 Se 55 (IG2):
1. Designing a super-structure surface structure with a vortex light generation function according to parameters such as refractive index of IG2 glass, and transferring the super-structure surface structure onto an upper mold core of a mold pressing mold;
2. cutting and cleaning spherical IG2 glass as a preform;
3. putting the preform into the center of a lower mold core of a clean precision mold pressing die, sleeving the lower mold core on a mold sleeve, and putting the upper mold core into the mold sleeve;
4. placing the precision mould pressing die into mould pressing equipment, and heating to 390 ℃ at the speed of 1 ℃/min;
5. applying a pressure to the mold at a rate of 1N/s to 600N;
6. maintaining the pressure and temperature for 30min;
7. reducing the pressure at 5N/min and reducing the temperature at 2 ℃/min;
8. stopping pressing when the temperature is lowered to 200 ℃;
9. cooling to 35 ℃ at a speed of 1 ℃/min, and taking out the vortex light generator with the super-structured surface;
10. the spherical chalcogenide glass polarization converter was annealed at 310 ℃ for 20h.
The plane IG2 glass vortex light generator with the super-structured surface is prepared by the embodiment, the appearance of the device is good, and the requirements of finished products of the vortex light generator are met.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions deviate from the technical solutions of the embodiments of the present invention.

Claims (10)

1. The preparation method of the high-precision molded sulfur optical device with the super-structure surface structure is characterized by comprising the following steps of:
firstly, transferring a designed super-structure surface structure pattern to a mould pressing mould core;
step two, pretreating a sulfur system preform;
thirdly, placing the pretreated chalcogenide preform into the center of a lower mold core of a precise mold pressing mold, sleeving the lower mold core into a mold sleeve, and then placing an upper mold core into the mold sleeve;
placing the precision mould pressing mould into mould pressing equipment, and slowly heating;
step five, performing mould pressing operation when the temperature is raised to a preset temperature above the glass transition temperature of the chalcogenide glass, and transferring the super-surface structure pattern on the mould core to the surface of the chalcogenide glass;
step six, keeping the pressure and the temperature for a preset time;
step seven, slowly reducing the pressure and cooling;
step eight, stopping applying the pressure when the temperature is lower than the glass transition temperature of the chalcogenide glass;
and step nine, slowly cooling to the discharging temperature to obtain the chalcogenide glass optical component with the super-structure surface.
2. The method of claim 1, wherein the patterned microstructured surface is one-sided or two-sided.
3. The method for producing a high-precision press-molded sulfur-based optical device having a super-textured surface structure according to claim 1, wherein a sulfur-based preform is a sheet-like or spherical sulfur-based preform.
4. The method of claim 1, wherein the temperature rise rate of the molding apparatus is not greater than 10 ℃/s, and the temperature drop rate of the molding apparatus is not greater than 10 ℃/s.
5. The method for producing a high-precision molded sulfur-based optical device with a super-structured surface structure according to claim 1, wherein the temperature at which the application of the pressure is started is not less than 5 ℃ higher than the glass transition temperature of the sulfur-based glass, and the temperature at which the application of the pressure is stopped is not more than 5 ℃ lower than the glass transition temperature of the sulfur-based glass.
6. The method of manufacturing a high-precision molded chalcogenide optical element having a metamaterial surface structure as claimed in claim 1, wherein the molding pressure is not greater than 10000N.
7. The method of claim 1, wherein the holding pressure and temperature are maintained for a period of time of no less than 5 seconds.
8. The method of making a high-precision molded, nanostructured surface structured sulfur-based optical device according to claim 1, wherein the discharge temperature is no greater than 100 ℃.
9. The method of making a high-precision molded, nanostructured surface structured sulfur-based optical device according to claim 1, further comprising: and annealing the chalcogenide glass optical component with the super-structured surface at the annealing temperature of not less than 50 ℃ for not less than 10min.
10. A high precision molded, nanostructured chalcogenide optical device prepared according to the method of any of claims 1-9.
CN202211317785.6A 2022-10-26 2022-10-26 High-precision molded sulfur optical device with super-structure surface structure and preparation method thereof Pending CN115536251A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101061058A (en) * 2004-05-24 2007-10-24 新加坡科技研究局 Imprinting of supported and free-standing 3-D micro-or nano-structures
CN107561857A (en) * 2017-09-20 2018-01-09 南方科技大学 A kind of method that the super structure surface of optics is prepared based on nano impression
US20190210915A1 (en) * 2018-01-09 2019-07-11 Chung-Ang University Industry-Academic Cooperation Foundation Glassy carbon roll-type mold manufacturing method for fine pattern formation, and glassy carbon roll-type mold manufactured by the method
CN111825311A (en) * 2019-04-17 2020-10-27 中国兵器工业第五九研究所 Micro-nano hot-press molding process for optical glass array lens
CN113740940A (en) * 2021-09-06 2021-12-03 长春理工大学 Wide-bandwidth angle anti-reflection composite micro-nano structure surface and preparation method thereof
CN113770668A (en) * 2021-10-13 2021-12-10 湖南大学 Method for preparing optical glass super-hydrophobic functional surface by utilizing hot press molding
CN114402251A (en) * 2019-07-29 2022-04-26 目立康株式会社 System and method for forming an ophthalmic lens comprising a superstructural optic

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101061058A (en) * 2004-05-24 2007-10-24 新加坡科技研究局 Imprinting of supported and free-standing 3-D micro-or nano-structures
CN107561857A (en) * 2017-09-20 2018-01-09 南方科技大学 A kind of method that the super structure surface of optics is prepared based on nano impression
US20190210915A1 (en) * 2018-01-09 2019-07-11 Chung-Ang University Industry-Academic Cooperation Foundation Glassy carbon roll-type mold manufacturing method for fine pattern formation, and glassy carbon roll-type mold manufactured by the method
CN111825311A (en) * 2019-04-17 2020-10-27 中国兵器工业第五九研究所 Micro-nano hot-press molding process for optical glass array lens
CN114402251A (en) * 2019-07-29 2022-04-26 目立康株式会社 System and method for forming an ophthalmic lens comprising a superstructural optic
CN113740940A (en) * 2021-09-06 2021-12-03 长春理工大学 Wide-bandwidth angle anti-reflection composite micro-nano structure surface and preparation method thereof
CN113770668A (en) * 2021-10-13 2021-12-10 湖南大学 Method for preparing optical glass super-hydrophobic functional surface by utilizing hot press molding

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Application publication date: 20221230