CN117626442A - Quinoline birefringent crystal, and preparation method and application thereof - Google Patents
Quinoline birefringent crystal, and preparation method and application thereof Download PDFInfo
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- CN117626442A CN117626442A CN202311642115.6A CN202311642115A CN117626442A CN 117626442 A CN117626442 A CN 117626442A CN 202311642115 A CN202311642115 A CN 202311642115A CN 117626442 A CN117626442 A CN 117626442A
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- 239000013078 crystal Substances 0.000 title claims abstract description 161
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 230000003287 optical effect Effects 0.000 claims abstract description 25
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000003755 preservative agent Substances 0.000 description 12
- 230000002335 preservative effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 230000010287 polarization Effects 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 238000001459 lithography Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 210000001747 pupil Anatomy 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses three quinoline birefringent crystals, a preparation method thereof and application thereof in a birefringent device. The chemical formula of the crystal material is shown as (C 9 H 6 BrN) X, wherein X is selected from the group consisting of hydrohalic acid or nitric acid; the quinoline birefringent crystal belongs to a cubic crystal system P2 1 /c or monoclinic system P2 1 And/m. The ultraviolet absorption cut-off side length of the crystal material is about 370nm, the birefringence of the crystal material at 550nm is 0.3-0.4, and the crystal material is a birefringent crystal material with potential application value and can be used for manufacturing FIR filters, optical isolators and beam positionsBirefringent optical devices such as movers, optical polarizers, and optical modulators.
Description
Technical Field
The invention relates to three quinoline birefringent crystals, a preparation method thereof and application thereof in preparation of birefringent devices.
Background
The birefringent crystal is an important photoelectric functional material and is widely applied to the technical and scientific research fields such as laser polarization technology, optical communication, polarization information processing, high-precision scientific research instruments and the like. The polarization state of the light can be modulated and detected by utilizing the birefringent crystal, and a polarizer, an analyzer, a polarizing beam splitter, an optical isolator, a circulator, a beam shifter, a phase retarder, an optoelectronic modulator and the like can be prepared. Depending on the absorption cut-off edge of the crystal, birefringent crystals may be applied in the ultraviolet (< 400 nm), visible (400-760 nm), infrared (> 760 nm) regions. As the laser application range expands toward short wavelength, the application of birefringent crystals in the ultraviolet deep ultraviolet region is also increasing. Of particular interest is the important application of birefringent crystals in the 193nm laser lithography field. The laser lithography technology is an indispensable process for large-scale and ultra-large-scale integrated circuits, however, in the process of implementing lithography, the polarization state of laser light is seriously affected and changed after passing through optical paths such as reflection, transmission, refraction and the like, which greatly weakens the resolution of lithography, and the polarization device made of birefringent crystal can modulate and detect the polarization state of the laser light, thereby improving the resolution of the lithography technology. For example, in 193nmArF lithography machine polarized illumination systems, measurement and control of illumination pupil polarization states is a critical technique that is necessary, and polarization devices made from birefringent crystals are core devices for measuring and controlling polarization states.
Currently, commercial birefringent crystals are mainly YV0 4 Iceberg (CaCO) 3 )、LiNbO 3 Rutile (TiO) 2 )、a-BaB 2 O 4 (a-BBO) and MgF 2 Isouniaxial crystals. YVO 4 Is an artificial birefringent crystal with good performance, and can easily grow high optical quality crystal by Czochralski method, but its transmission range is 400-5000nm, and can not be used in ultraviolet region. The icelandite crystal is mainly obtained from natural minerals, is a non-renewable resource, is difficult to artificially synthesize, has smaller general size, and cannot meet the requirements of large-size optical polarizing elements. LiNbO 3 Crystals are easy to obtain largeSize crystals, but their low birefringence is disadvantageous for device miniaturization in practical applications. Rutile has a very large birefringence, but it is not prone to large-size crystal growth and the difficulty of processing devices is great due to its high hardness. The a-BBO is an artificially synthesized birefringent crystal with excellent performance, has a larger birefringent index, a high laser damage threshold value and a wide light transmission range, can be widely applied to near infrared, visible light and ultraviolet light bands, can be used for a high-power laser system, and is the only birefringent crystal material with large birefringent index available in the ultraviolet region. However, due to the existence of solid phase transition, the a-BBO crystal is easy to crack in the growth process, and although the phase transition can be restrained by a doping method, the quality of the crystal can be reduced along with doping, and the crystal with high optical quality is not easy to obtain; meanwhile, a-BBO is difficult to apply to deep ultraviolet band due to the limitation of transmission range, and in addition, a-BBO crystals have moisture absorption, which affects the optical quality of the crystals. MgF (MgF) 2 The crystal is a birefringent material with excellent deep ultraviolet performance, has been well applied to 193nm lithography and other basic research fields, however, the birefringence is too small to be used for manufacturing a gram-Taylor prism, and can only be used for manufacturing a Rochon prism, a Wollaston prism and the like, and the beam separation angle is small, the size of a device is large, and the use is inconvenient. In addition, currently commercialized birefringent crystals are all uniaxial crystals, and there is little research on biaxial birefringent crystals. Therefore, there is a great need to find new birefringent crystal materials that can overcome the deficiencies of existing birefringent crystals.
Disclosure of Invention
The invention aims to provide three quinoline birefringent crystals, a preparation method thereof and application thereof in a birefringent instrument.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the first to be protected of the present invention are three kinds of quinoline birefringent crystals.
1) First quinoline birefringent crystal (C 9 H 6 BrN). HBr, which belongs to cubic system P2 1 Space group/c, its crystal structure is lamellar structure, and unit cell parameter isα＝90.00°，β＝98.788°，γ＝90.00°，/>Z＝4。
2) Second quinoline birefringent crystal (C 9 H 6 BrN). HCl, belonging to cubic system P2 1 Space group/c, its crystal structure is lamellar structure, and unit cell parameter isα＝90.00°，β＝97.922°，γ＝90.00°，/>Z＝4。
3) Third quinoline birefringent crystal (C 9 H 6 BrN)·HNO 3 Belonging to monoclinic system P2 1 The m space group has a layered crystal structure and unit cell parameters ofβ＝108.379°，γ＝90.00°，/>Z＝2
The second to be protected of the invention is a preparation method of the three kinds of quinoline birefringent crystals, which is to prepare the three kinds of quinoline birefringent crystals by adopting an aqueous solution evaporation method; preparation method of quinoline birefringent crystal C 9 H 6 BrN, halogen acid or nitric acid and deionized water are used as raw materials, and water solution evaporation is used for preparing the quinoline birefringent crystal.
Preparation of first quinoline birefringent Crystal (C) by aqueous solution evaporation 9 H 6 BrN). HBr, the specific steps are as follows: c is C 9 H 6 BrN (1 mL), HBr (10 mL), deionized water (10 mL) were mixed in a glass beaker, and the beaker sealed with a preservative film was heated at 348-373KStirring with a magnetic stirrer until the solution is clear and transparent. The beaker is sealed by a preservative film with holes, the beaker is placed at 300-333K for one day to enable colorless lamellar crystals to be precipitated at the bottom of the beaker, and then the purity of the crystals of the product is confirmed by measuring an X-ray diffraction pattern of the crystals.
The quinoline birefringent crystal prepared by the preparation method has the advantages of stable physical property, good thermal stability, high growth speed, more convenient processing and the like.
Preparation of a second quinoline birefringent Crystal (C) by aqueous solution evaporation 9 H 6 BrN). HCl, the specific steps are: c is C 9 H 6 BrN (1 mL), HCl (10 mL), deionized water (10 mL) were mixed in a glass beaker, and then the beaker sealed with a preservative film was heated at 348-373K and stirred with a magnetic stirrer until the solution was clear and transparent. The beaker is sealed by a preservative film with holes, the beaker is placed at 300-333K for a few days to enable colorless lamellar crystals to be precipitated at the bottom of the beaker, and then the purity of the crystals of the product is confirmed by measuring an X-ray diffraction pattern of the crystals.
The quinoline birefringent crystal prepared by the preparation method has the advantages of stable physical property, good thermal stability, high growth speed, more convenient processing and the like.
Preparation of a third quinoline birefringent Crystal (C) by aqueous solution evaporation 9 H 6 BrN)·HNO 3 The method comprises the following specific steps: c is C 9 H 6 BrN(1mL)，HNO 3 (10 mL), deionized water (10 mL) was mixed in a glass beaker, and the beaker sealed with a preservative film was heated at 348-373K and stirred with a magnetic stirrer until the solution was clear and transparent. The beaker is sealed by a preservative film with holes, the beaker is placed at 300-333K for a few days to enable colorless lamellar crystals to be precipitated at the bottom of the beaker, and then the purity of the crystals of the product is confirmed by measuring an X-ray diffraction pattern of the crystals.
The quinoline birefringent crystal prepared by the preparation method has the advantages of stable physical property, good thermal stability, high growth speed, more convenient processing and the like.
The third aspect of the present invention is the application of the three kinds of quinoline birefringent crystals in preparing birefringent devices. The birefringent device is an optical FIR filter or the like.
Preferably, the birefringent device operates according to the following principle: after at least one linearly polarized light is passed through at least two quinoline birefringent crystals, two light beams having a time difference are outputted due to the difference in time of passing through the crystals, and two light beams split along the fast-fast axis and the slow-slow axis are formed in time of passing through the second birefringent crystal one each.
The invention has the beneficial effects that: the three quinoline birefringent crystals obtained by the invention have the advantages of stable physical properties, good thermal stability, high growth speed, more convenient processing and the like; can be used for manufacturing an optical FIR filter, an optical isolator, a light beam shifter, an optical polarizer, an optical modulator and the like
Drawings
FIG. 1 shows a first quinoline birefringent crystal (C) 9 H 6 Crystal structure diagram of BrN). HBr, second quinoline birefringent Crystal (C) prepared in example 2 9 H 6 Crystal structure diagram of BrN). HCl and third quinoline birefringent Crystal (C) prepared in example 3 9 H 6 BrN)·HNO 3 Is a crystal structure diagram of (a).
FIG. 2 shows a first quinoline birefringent crystal (C 9 H 6 BrN). Pure phase XRD alignment pattern of HBr, second quinoline birefringent Crystal (C) prepared in example 2 9 H 6 Pure-phase XRD alignment pattern for BrN). HCl and the third quinoline birefringent crystal (C) prepared in example 3 9 H 6 BrN)·HNO 3 Pure phase XRD comparison pattern of (c).
FIG. 3 shows a first quinoline birefringent crystal (C) 9 H 6 BrN). HBr, a second quinoline birefringent crystal (C) prepared in example 2 9 H 6 BrN). HCl ultraviolet-visible light diffuse reflectance Spectrum and third quinoline birefringent Crystal (C) prepared in example 3 9 H 6 BrN)·HNO 3 Is a diffuse reflection spectrum of ultraviolet-visible light.
Fig. 4 is a schematic diagram of the operation of a typical birefringent device using three kinds of quinoline birefringent crystals prepared in example 1, example 2 and example 3, wherein E is a laser emitter, P is a polarizer, and C is a quinoline crystal subjected to post-crystal treatment and optical processing.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
EXAMPLE 1 preparation of first quinoline Crystal
Preparation of the first quinoline birefringent Crystal (C) by aqueous solution evaporation 9 H 6 BrN). HBr, C 9 H 6 BrN (1 mL), HBr (10 mL), deionized water (10 mL) were mixed in a glass beaker, and then heated at 373K with a preservative film sealed beaker and stirred with a magnetic stirrer until the solution was clear and transparent. The beaker was sealed with a perforated preservative film and allowed to stand at 300K for one day to precipitate colorless layered crystals at the bottom of the beaker, after which the crystal purity was confirmed by measuring the X-ray diffraction pattern of the crystals.
Through testing (figure 1), the prepared quinoline crystal birefringent crystal does not contain a symmetrical center and belongs to a cubic crystal system P2 1 Space group/c, whose unit cell parameters areα＝90.00°，β＝98.788°，γ＝90.00°，/>Z＝4。
The obtained quinoline birefringent crystal is subjected to XRD pure phase contrast test (figure 2), and the XRD spectrum of the crystal is better matched with that of a single crystal XRD analysis and calculation.
The obtained quinoline birefringent crystal is subjected to ultraviolet-visible light diffuse reflection spectrum test (figure 3), and the ultraviolet absorption cut-off edge of the crystal is 375nm.
The obtained quinoline birefringent crystal is subjected to a birefringent index test, and the birefringent index delta n=0.328@550nm of the crystal is measured, so that the crystal has more excellent performance compared with other birefringent crystals on the market.
The obtained quinoline birefringent crystal is applied to an optical device, a structural schematic diagram (figure 4) is drawn, at room temperature, a laser emits line laser to irradiate a first crystal through a polaroid to generate two beams of light rays of a fast axis and a slow axis, then four beams of light are generated through a second fast crystal, and finally the four beams of light rays are filtered through the polaroid to form three medium-frequency beams of the fast axis, the slow axis and the slow axis.
EXAMPLE 2 preparation of the second quinoline Crystal
Preparation of the second quinoline birefringent Crystal (C) by aqueous solution evaporation 9 H 6 BrN). HCl, C 9 H 6 BrN (1 mL), HCl (10 mL), deionized water (10 mL) were mixed in a glass beaker, and then heated at 373K with a preservative film sealed beaker and stirred with a magnetic stirrer until the solution was clear and transparent. The beaker was sealed with a perforated preservative film and allowed to stand at 300K for one day to precipitate colorless layered crystals at the bottom of the beaker, after which the crystal purity was confirmed by measuring the X-ray diffraction pattern of the crystals.
Through testing (figure 1), the prepared quinoline crystal birefringent crystal does not contain a symmetrical center and belongs to a cubic crystal system P2 1 Space group/c, its crystal structure is lamellar structure, and unit cell parameter is α＝90.00°，β＝97.922°，γ＝90.00°，/>Z＝4。
The obtained quinoline birefringent crystal is subjected to XRD pure phase contrast test (figure 2), and the XRD spectrum of the crystal is better matched with that of a single crystal XRD analysis and calculation.
The obtained quinoline birefringent crystal was subjected to an ultraviolet-visible light diffuse reflection spectrum test (FIG. 3), and the ultraviolet absorption cut-off edge of the crystal was found to be 370nm.
The obtained quinoline birefringent crystal is subjected to a birefringent index test, and the birefringent index delta n=0.277@550nm of the crystal is measured, so that the crystal has more excellent performance compared with other birefringent crystals on the market.
The obtained quinoline birefringent crystal is applied to an optical device, a structural schematic diagram (figure 4) is drawn, at room temperature, a laser emits line laser to irradiate a first crystal through a polaroid to generate two beams of light rays of a fast axis and a slow axis, then four beams of light are generated through a second fast crystal, and finally the four beams of light rays are filtered through the polaroid to form three medium-frequency beams of the fast axis, the slow axis and the slow axis.
EXAMPLE 3 preparation of third quinoline Crystal
Preparation of the third quinoline birefringent Crystal (C) by aqueous solution evaporation 9 H 6 BrN)·HNO 3 C is carried out by 9 H 6 BrN(1mL),HNO 3 (10 mL), deionized water (10 mL) was mixed in a glass beaker, and then the beaker was heated at 373K with a preservative film seal, and stirred with a magnetic stirrer until the solution was clear and transparent. The beaker was sealed with a perforated preservative film and allowed to stand at 300K for one day to precipitate colorless layered crystals at the bottom of the beaker, after which the crystal purity was confirmed by measuring the X-ray diffraction pattern of the crystals.
Through testing (figure 1), the prepared quinoline crystal birefringent crystal does not contain a symmetrical center and belongs to monoclinic system P2 1 The m space group has a layered crystal structure and unit cell parameters of α＝90.00°，β＝108.379°，γ＝90.00°，/>Z＝2。
The obtained quinoline birefringent crystal is subjected to XRD pure phase contrast test (figure 2), and the XRD spectrum of the crystal is better matched with that of a single crystal XRD analysis and calculation.
The obtained quinoline birefringent crystal was subjected to an ultraviolet-visible light diffuse reflection spectrum test (FIG. 3), and the ultraviolet absorption cut-off edge of the crystal was found to be 370nm.
The obtained quinoline birefringent crystal is subjected to a birefringent index test, and the birefringent index delta n=0.401@550nm of the crystal is measured, so that the crystal has more excellent performance compared with other birefringent crystals on the market.
The obtained quinoline birefringent crystal is applied to an optical device, a structural schematic diagram (figure 4) is drawn, at room temperature, a laser emits line laser to irradiate a first crystal through a polaroid to generate two beams of light rays of a fast axis and a slow axis, then four beams of light are generated through a second fast crystal, and finally the four beams of light rays are filtered through the polaroid to form three medium-frequency beams of the fast axis, the slow axis and the slow axis.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (9)
1. A quinoline birefringent crystal has a chemical formula (C 9 H 6 BrN). X, wherein X is selected from the group consisting of hydrohalic acid or nitric acid; the quinoline birefringent crystal belongs to a cubic crystal system P2 1 /c or monoclinic system P2 1 /m。
2. The quinoline birefringent crystal according to claim 1, wherein the quinoline birefringent crystal is (C 9 H 6 BrN). HBr, which belongs to cubic system P2 1 The unit cell parameters of/c are a= 7.7945 a, b= 16.9033 a, c= 7.3435 a, α=90.00°, β= 98.788 °, γ=90.00°, v= 956.17 a 3, z=4.
3. The quinoline birefringent crystal according to claim 1, wherein the quinoline birefringent crystal is (C 9 H 6 BrN). HCl, belonging to cubic system P2 1 The unit cell parameters of/c are a= 7.6689 a, b= 16.5241 a, c= 7.3371 a, α=90.00°, β= 97.922 °, γ=90.00°, v= 920.90 a 3, z=4.
4. The quinoline birefringent crystal according to claim 1, wherein the quinoline birefringent crystal is (C 9 H 6 BrN)·HNO 3 Belonging to monoclinic system P2 1 /m, the unit cell parameters area=8.9883Å，b=6.2977Å，c=9.2738Å，α= 90.00°，β=108.379°，γ=90.00°，V=498.17Å 3 ，Z=2。
5. The method for producing a quinoline birefringent crystal according to any one of claims 1 to 4, wherein: evaporating the aqueous solution to obtain C 9 H 6 And (3) mixing BrN, halogen acid or nitric acid and deionized water, heating, standing, cooling and crystallizing to obtain the quinoline birefringent crystal.
6. The method of claim 5, wherein C 9 H 6 The volume ratio of BrN, halogen acid or nitric acid and deionized water is (1-3) ml: (10-20) ml: (10-20) ml; the heating temperature is 348-373K; the standing cooling temperature is 300-333K.
7. Use of a quinoline birefringent crystal according to any one of claims 1 to 4 as a birefringent optical device.
8. The use according to claim 7, wherein: the birefringent optical component is an FIR filter, an optical isolator, a beam shifter, a circulator, an optical isolator or an optical modulator.
9. An FIR filter comprising the quinoline birefringent crystal according to any one of claims 1 to 4.
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