CN117865073A - Compound sodium vanadium selenite, compound sodium vanadium selenite birefringent crystal, preparation method and application - Google Patents
Compound sodium vanadium selenite, compound sodium vanadium selenite birefringent crystal, preparation method and application Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 130
- 150000001875 compounds Chemical class 0.000 title claims abstract description 88
- -1 sodium vanadium selenite Chemical compound 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 41
- 230000003287 optical effect Effects 0.000 claims abstract description 39
- 238000007789 sealing Methods 0.000 claims abstract description 25
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000004891 communication Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000011734 sodium Substances 0.000 claims description 51
- 239000010453 quartz Substances 0.000 claims description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 44
- 238000001816 cooling Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 15
- 238000009461 vacuum packaging Methods 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000005538 encapsulation Methods 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005520 cutting process Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000012071 phase Substances 0.000 description 12
- 238000000227 grinding Methods 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 8
- 238000006757 chemical reactions by type Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000001902 propagating effect Effects 0.000 description 3
- 229910021532 Calcite Inorganic materials 0.000 description 2
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a compound sodium vanadium selenite, a compound sodium vanadium selenite optical crystal, a preparation method and application, wherein the chemical formula of the compound is NaVSeO 5 The molecular weight is 232.89, and the crystal is NaVSeO 5 The molecular weight is 232.89, the crystal belongs to monoclinic system and space groupC2/cThe unit cell parameters area=18.234(3)Å，b=3.8381(6)Å，c=12.416(2)Å，α=90°，β=112.421(7)°，γ=90°，V=803.2(2)Å 3 Z=8. By usingAnd (3) growing crystals by a sealed molten salt method, a high-temperature molten liquid method or a vacuum tube sealing method. At a wavelength of 1064nm, the crystal has a birefringence Δn=0.12, good chemical stability, moderate mechanical hardness, easy cutting, polishing, processing and storage, is insoluble in water, does not deliquescence, and is suitable for manufacturing polarizing prisms, phase retardation devices and electro-optical modulation devices for optical communication elements or various applications, such as a graticule prism, a polarizing beam splitter, a compensator, an optical isolator circulator, an optical modulator, and the like. Has important roles in the fields of optics and communication.
Description
Technical Field
The invention relates to a catalyst with a chemical formula of NaVSeO 5 Compounds of (2) and navso 5 Birefringent crystals, methods of making crystals and uses thereof.
Background
The birefringence phenomenon is one of the important characteristics exhibited by light propagating in a medium crystal whose optical properties are non-uniform, and the fundamental cause of this phenomenon is the anisotropy of the crystal material, which can be explained by the transverse wave nature of light. When light propagates through an optically non-homogeneous body (e.g., a crystal other than a cubic system), the vibration characteristics of the light are changed except for the specific directions (along the optical axis direction), and the light is decomposed into two polarized lights with two electric field vector vibration directions perpendicular to each other, different propagation speeds and different refractive indexes, and the phenomenon is called birefringence, and the crystal is called birefringent crystal. One of the two beams follows the general law of refraction, called ordinary light (o-light), and its refractive index is n o Meaning that the other beam does not follow the general law of refraction, called extraordinary light (e-light), its refractive index is defined by n e And (3) representing. Linearly polarized light can be obtained by utilizing the characteristics of the birefringent crystal, and displacement and the like of light beams are realized. Therefore, the birefringent crystal is a key material for manufacturing optical elements such as an optical isolator, an circulator, a beam shifter, an optical polarizer, an optical modulator and the like.
The common birefringent materials are mainly calcite, rutile and LiNbO 3 、YVO 4 alpha-BaB 2 O 4 Crystals, and the like. However, calcite crystals mainly exist in natural forms, and artificial synthesis is difficult; the optical polarizing element has the advantages of smaller general size, higher impurity content, difficulty in processing and low crystal utilization rate, and can not meet the requirements of large-size optical polarizing elements, and is easy to dissociate. Rutile also exists mainly in natural form, is difficult to synthesize artificially, and is small in size, large in hardness and difficult to process. LiNbO 3 Crystals tend to give large-sized crystals, but the birefringence is too small. YVO 4 Is a person with good performanceAn artificial birefringent crystal, but due to YVO 4 The melting point is high, the iridium crucible is required to be used for carrying out pulling growth, and the growth atmosphere is a weak oxygen atmosphere, so that the problem of price change of iridium element during growth is solved, and high-quality crystals are not easy to obtain. alpha-BaB 2 O 4 Due to the existence of solid phase transformation, cracking is easy during crystal growth. In view of this, it is highly necessary to find a birefringent crystal which is easy to grow, stable in performance, and has a large birefringence.
Disclosure of Invention
The invention aims to provide a sodium vanadium selenite compound, which has a chemical formula of NaVSeO 5 The molecular weight is 232.89, and the preparation method is vacuum encapsulation method.
Another object of the present invention is to provide sodium vanadium selenite birefringent crystal of the formula NaVSeO 5 The molecular weight is 232.89, the crystal belongs to monoclinic system, the space group C2/C is that the unit cell parameter is α＝90°，β＝112.421(7)°，γ＝90°，/>Z＝8。
The invention also aims to provide a preparation method of the sodium vanadium selenite birefringent crystal, which adopts a sealed molten salt method to grow the crystal by a high Wen Rongye-degree or vacuum packaging method.
It is still another object of the present invention to provide a use of the sodium vanadium selenite optical birefringent crystal for fabricating optical communication elements, i.e., optical isolators, circulators, beam displacers, optical polarizers and optical modulators, particularly for fabricating polarizing prisms, phase delay devices and electro-optic modulation devices for various uses.
The chemical formula of the compound sodium vanadium selenite is NaVSeO 5 Molecular weight 232.89, trueAnd (5) preparing by an empty packaging method.
The preparation method of the compound sodium vanadium selenite adopts a vacuum packaging method, and the specific operation is carried out according to the following steps:
uniformly mixing Na-containing compound, V-containing compound and Se-containing compound according to the molar ratio of Na to V to Se=1:1:1, filling into quartz tube, and vacuum-pumping the quartz tube to vacuum degree of 10 -3 Sealing at Pa and high temperature, placing in a muffle furnace, heating to 200-550deg.C at a rate of 5-10deg.C/h, and keeping constant temperature for 24-100 hr to obtain NaVSeO 5 The Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
Sodium vanadium selenite birefringent crystal with chemical formula of NaVSeO 5 The molecular weight is 232.89, the crystal belongs to monoclinic system, the space group C2/C is that the unit cell parameter isα＝90°，β＝112.421(7)°，γ＝90°，/>Z＝8。
The preparation method of the sodium vanadium selenite birefringent crystal adopts a sealed molten salt method, and grows the crystal by a high Wen Rongye method or a vacuum packaging method, wherein:
the sealed molten salt growth NaVSeO 5 The birefringent crystal is prepared by the following steps:
a. uniformly mixing a Na-containing compound, a V-containing compound and a Se-containing compound according to the molar ratio of Na to V to Se=1 to 1, transferring into a lining of a high-pressure hydrothermal kettle, and sealing the high-pressure hydrothermal kettle, wherein the Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
b. Heating to 300-550deg.C at a rate of 5-10deg.C/h, maintaining the temperature for 2-3 days, slowly cooling to room temperature at a rate of 1-5deg.C/d, and opening the high pressure hydrothermal kettle to obtain NaVSeO 5 A birefringent crystal;
NaVSeO is prepared by the high-temperature melt method 5 The birefringent crystal is prepared by the following steps:
a. uniformly mixing Na-containing compound, V-containing compound and Se-containing compound according to the molar ratio of Na to V to Se=1 to 1, placing into a quartz tube, vacuumizing the quartz tube, and keeping the vacuum degree to 10 -3 Sealing at high temperature of Pa, placing in a muffle furnace, heating to 200-550deg.C at a speed of 5-10deg.C/h, and keeping constant temperature for 24-100 hr to obtain NaVSeO 5 The Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
b. Subjecting the compound NaVSeO obtained in step a to 5 Placing the mixture into a corundum crucible, heating to 450-600 ℃, and keeping the temperature for 5-100 hours to obtain mixed melt;
c. preparing seed crystals: c, placing the mixed solution obtained in the step b into a single crystal furnace, slowly cooling to 220 ℃ at the speed of 0.1-2 ℃/h, and rapidly cooling to room temperature at the speed of 5-10 ℃/h to obtain NaVSeO 5 Seed crystal;
d. growing a crystal: c, fixing the seed crystal obtained in the step c on a seed rod, applying 2-20rpm of crystal rotation from the upper side of the mixed solution obtained in the step b through a crystal growth controller, cooling at a speed of 0.1-3 ℃/h, and obtaining NaVSeO after the crystal growth is stopped 5 A birefringent crystal;
the vacuum packaging method prepares NaVSeO 5 The birefringent crystal is prepared by the following steps:
a. na-containing compound, V-containing compound and Se-containing compound are added in a molar ratio of Na:V:Se=1:1:1Mixing, placing into quartz tube, vacuumizing the quartz tube to vacuum degree of 10 -3 Sealing at high temperature of Pa, placing in a muffle furnace, heating to 200-550deg.C at a speed of 5-10deg.C/h, and keeping constant temperature for 24-100 hr to obtain NaVSeO 5 The Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
b. The NaVSeO obtained in the step a is treated 5 Placing the polycrystalline powder into a quartz tube, sealing at high temperature, placing into a muffle furnace, heating to 450-600deg.C, maintaining the temperature for 50-100 hr, cooling to 220deg.C at a rate of 0.1-3deg.C/h, and rapidly cooling to room temperature at a rate of 5-10deg.C/h to obtain NaVSeO 5 Birefringent crystals.
The sodium vanadium selenite birefringent crystal is used for preparing optical communication elements, namely an optical isolator, an circulator, a beam shifter, an optical polarizer or an optical modulator.
The sodium vanadium selenite optical crystal is used for manufacturing various polarizing prisms, namely a phase delay device and an electro-optic modulation device.
The sodium vanadium selenite birefringent crystal obtained by the method has moderate mechanical hardness and is easy to cut, polish, process and store. Is insoluble in water, does not deliquesce, is stable in air, and is suitable for manufacturing optical communication elements such as optical isolators, circulators, beam displacers, optical polarizers, optical modulators and the like. Is especially suitable for making polarizing prisms, phase delay devices and electro-optic modulation devices for various purposes.
Drawings
FIG. 1 shows NaVSeO of the present invention 5 X-ray diffraction pattern of the powder;
FIG. 2 is a NaVSeO of the present invention 5 A crystallography map;
FIG. 3 is a NaVSeO of the present invention 5 A crystal structure diagram;
FIG. 4 is a NaVSeO of the present invention 5 A birefringence profile;
FIG. 5 is a schematic diagram of a wedge-shaped birefringent crystal polarizing beam splitter of the present invention, wherein 1 is incident light, 2 is o light, 3 is e light, 4 is optical axis, and 5 is NaVSeO 5 A crystal;
FIG. 6 is a schematic view of an optical isolator according to the present invention, wherein 6 is the transmission direction;
FIG. 7 is a schematic diagram of a beam shifter according to the present invention, wherein 1 is incident light, 2 is o light, and 3 is e light NaVSeO 5 Crystal, 4 is optical axis, 5 is NaVSeO 5 Crystal, 6 light transmission direction, 7 optical axis surface.
Detailed Description
The invention is further described below with reference to examples. It should be noted that the following examples should not be construed as limiting the scope of the invention, and any modifications made thereto do not depart from the spirit of the invention. The materials and equipment used in the present invention are commercially available unless otherwise specified.
Example 1
According to the reaction formula: na (Na) 2 SO 4 +V 2 O 5 +2SeO 2 →2NaVSeO 5 +SO 3 ∈, preparing NaVSeO compound by vacuum encapsulation method 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction formula, na 2 SO 4 、V 2 O 5 And SeO 2 Mixing uniformly, and grinding in a mortar for 15 minutes to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 400 ℃ at the speed of 10 ℃/h, keeping the temperature for 25 hours, cooling to room temperature, closing the muffle furnace, taking out a sample after cooling, and obtaining a compound NaVSeO 5 。
Example 2
According to the reaction formula: 2NaOH+V 2 O 5 +2SeO 2 →2NaVSeO 5 +H 2 O ≡preparation of compound Na by vacuum packaging methodVSeO 5 The specific operation is carried out according to the following steps:
a. NaOH and V are mixed according to the proportion in the reaction type 2 O 5 And SeO 2 Mixing uniformly, and then placing in a mortar, grinding for 15 minutes to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 350 ℃ at a speed of 5 ℃/h, preserving heat for 72 days, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 3
According to the reaction formula: 4NaNO 3 +2V 2 O 5 +4SeO 2 →4NaVSeO 5 +4NO 2 ↑+O 2 ∈, preparing NaVSeO compound by vacuum encapsulation method 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction type, naNO is prepared 3 、V 2 O 5 And SeO 2 Mixing uniformly, and grinding in a mortar for 13 minutes to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. c, placing the quartz tube in the step b into a muffle furnace, and heating to 330 ℃ at a speed of 7 ℃/h; preserving heat for 72 hours, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 4:
according to the reaction formula: 4Na 2 O+2V 2 O 5 +4SeO 2 →4NaVSeO 5 +O 2 ∈, preparing NaVSeO compound by vacuum encapsulation method 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction formula, na 2 O、V 2 O 5 And SeO 2 Mixing uniformly, and grinding for 20 minutes in a mortar to obtain a mixture;
b. in step aFilling the mixture into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 350 ℃ at the speed of 6 ℃/h, preserving heat for 40 hours, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 5
According to the reaction formula: naVO (NaVO) 3 +SeO 2 →NaVSeO 5 Vacuum packaging method for preparing NaVSeO compound 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction type, naVO is added 3 And SeO 2 Mixing uniformly, and grinding for 20 minutes in a mortar to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 400 ℃ at the speed of 10 ℃/h, preserving heat for 72 hours, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 6
According to the reaction formula: na (Na) 2 CO 3 +V 2 O 5 +2SeO 2 →2NaVSeO 5 +CO 2 ∈, preparing NaVSeO compound by vacuum encapsulation method 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction formula, na 2 CO 3 、V 2 O 5 And SeO 2 Mixing uniformly, and grinding for 20 minutes in a mortar to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 390 ℃ at the speed of 10 ℃/h, preserving heat for 25 hours, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 7
According to the reaction formula: na (Na) 2 CO 3 +V 2 O 5 +2H 2 SeO 4 →2NaVSeO 5 +2H 2 O↑+CO 2 ↑+O 2 ∈, preparing NaVSeO compound by vacuum encapsulation method 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction formula, na 2 CO 3 、V 2 O 5 And H 2 SeO 4 Mixing uniformly, and grinding for 20 minutes in a mortar to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 380 ℃ at the speed of 10 ℃/h, preserving heat for 30 hours, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 8
According to the reaction formula: 4NaNO 3 +2V 2 O 5 +4H 2 SeO 4 →4NaVSeO 5 +4H 2 O↑+4NO 3 ↑+O 2 ∈, preparing NaVSeO compound by vacuum encapsulation method 5 The specific operation is carried out according to the following steps:
a. according to the proportion in the reaction type, naNO is prepared 3 、V 2 O 5 And H 2 SeO 4 Mixing uniformly, and grinding for 20 minutes in a mortar to obtain a mixture;
b. c, filling the mixture obtained in the step a into a quartz tube with the diameter of 40mm, vacuumizing the quartz tube to reach the vacuum degree of 10 - 3 Sealing at high temperature after Pa;
c. putting the quartz tube in the step b into a muffle furnace, heating to 360 ℃ at the speed of 10 ℃/h, preserving heat for 50 hours, and then cooling to room temperature to obtain the compound NaVSeO 5 。
Example 9
Growth of NaVSeO by sealed molten salt method 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 1 5 Transferring the pure phase into a lining of the high-pressure hydrothermal kettle, and sealing the high-pressure hydrothermal kettle;
placing the high-pressure hydrothermal kettle in a baking oven, heating to 550 ℃ at the speed of 5 ℃/h, preserving heat for 24 hours, cooling to room temperature at the speed of 2 ℃/d, and opening the high-pressure hydrothermal kettle to obtain NaVSeO with the diameter of phi 6mm multiplied by 0.2mm multiplied by 0.3mm 5 Birefringent crystals.
Example 10
Growth of NaVSeO by sealed molten salt method 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 2 5 Transferring the pure phase into a lining of the high-pressure hydrothermal kettle, and sealing the high-pressure hydrothermal kettle;
placing the high-pressure hydrothermal kettle in a baking oven, heating to 600 ℃ at the speed of 6 ℃/h, controlling the furnace temperature to 600 ℃, preserving heat for 44 hours, cooling to room temperature at the speed of 5 ℃/d, and opening the high-pressure hydrothermal kettle to obtain NaVSeO with the diameter of phi 5mm multiplied by 0.2mm multiplied by 0.3mm 5 Birefringent crystals.
Example 11
Growth of NaVSeO by sealed molten salt method 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 3 5 Transferring the pure phase into a lining of the high-pressure hydrothermal kettle, and sealing the high-pressure hydrothermal kettle;
placing the high-pressure hydrothermal kettle in a baking oven, heating to 470 ℃ at the speed of 10 ℃/h, controlling the furnace temperature to 470 ℃, preserving heat for 24 hours, cooling to room temperature at the speed of 2 ℃/d, and opening the high-pressure hydrothermal kettle to obtain NaVSeO with the particle diameter phi of 5mm multiplied by 0.5mm multiplied by 0.4mm 5 Birefringent crystals.
Example 12
Growing NaVSeO by adopting high-temperature melt method 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 4 5 Pure phase is put into a corundum crucible, heated to 550 ℃ and kept at constant temperature for 50 hours to obtain mixed melt;
preparing seed crystals: placing the obtained mixed solution into a single crystal furnace, cooling to 220 ℃ at the speed of 0.1 ℃/h, and rapidly cooling to room temperature at the speed of 5 ℃/h to obtain NaVSeO 5 Seed crystal;
growing a crystal: fixing the obtained seed crystal on a seed rod, seeding the seed crystal from the upper part of the prepared mixed solution, applying 2rpm of crystal rotation through a crystal growth controller, cooling at the speed of 0.1 ℃/h, and obtaining NaVSeO with the size phi 3mm multiplied by 0.4mm multiplied by 1mm after the crystal growth is stopped 5 Birefringent crystals.
Example 13
Growing NaVSeO by adopting high-temperature melt method 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 5 5 Pure phase is put into a corundum crucible, heated to 450 ℃ and kept at constant temperature for 100 hours to obtain mixed melt;
preparing seed crystals: placing the obtained mixed solution into a single crystal furnace, cooling to 220 ℃ at the speed of 1 ℃/h, and rapidly cooling to room temperature at the speed of 8 ℃/h to obtain NaVSeO 5 Seed crystal;
growing a crystal: fixing the obtained seed crystal on a seed rod, seeding the seed crystal from the upper part of the prepared mixed solution, applying 20rpm crystal rotation by a crystal growth controller, cooling at a speed of 3 ℃/h, and obtaining NaVSeO with the size phi 4mm multiplied by 0.2mm multiplied by 1mm after the crystal growth is stopped 5 Birefringent crystals.
Example 14
Growing NaVSeO by adopting high-temperature melt method 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 5 5 Pure phase is put into a corundum crucible, heated to 600 ℃ and kept at constant temperature for 5 hours to obtain mixed melt;
preparing seed crystals: the obtained mixed solution is placed in a single crystal furnace, slowly cooled to 220 ℃ at the speed of 2 ℃/h, and then rapidly cooled to room temperature at the speed of 10 ℃/h, thus obtaining NaVSeO 5 Seed crystal;
growing a crystal: fixing the obtained seed crystal on seed rod, and obtaining mixed solutionSeeding above, applying 10rpm crystal rotation by a crystal growth controller, cooling at a rate of 1 ℃/h, and stopping crystal growth to obtain NaVSeO with a size of phi 5mm×0.3mm×0.4mm 5 Birefringent crystals.
Example 15
Vacuum packaging method for growing NaVSeO 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 6 5 Pure phase is filled into a quartz tube with the diameter of 40mm, the quartz tube is vacuumized, and the vacuum degree reaches 10 -3 Sealing at high temperature after Pa, heating to 500 ℃ in a muffle furnace, keeping the temperature for 72 hours, then cooling to 200 ℃ at the speed of 1 ℃/h, and then rapidly cooling to room temperature at the speed of 8 ℃/h to obtain NaVSeO with the size of phi 3mm multiplied by 0.5mm multiplied by 1mm 5 Birefringent crystals.
Example 16
Vacuum packaging method for growing NaVSeO 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 7 5 Pure phase is filled into a quartz tube with the diameter of 40mm, the quartz tube is vacuumized, and the vacuum degree reaches 10 -3 Sealing at high temperature after Pa, heating to 450 ℃, keeping the temperature for 100 hours, reducing to 200 ℃ at the speed of 0.1 ℃/h, and then rapidly cooling to room temperature at the speed of 10 ℃/h, namely NaVSeO with the size of phi 4mm multiplied by 0.3mm multiplied by 0.8mm 5 A birefringent crystal;
example 17
Vacuum packaging method for growing NaVSeO 5 The birefringent crystal is prepared by the following steps:
the compound NaVSeO obtained in example 8 5 Pure phase is filled into a quartz tube with the diameter of 40mm, the quartz tube is vacuumized, and the vacuum degree reaches 10 -3 Sealing at high temperature after Pa, placing into a muffle furnace, heating to 600 ℃, keeping the temperature for 50 hours, then cooling to 220 ℃ at the speed of 3 ℃/h, and then rapidly cooling to room temperature at the speed of 5 ℃/h, namely NaVSeO with the size of phi 4mm multiplied by 0.5mm multiplied by 2mm 5 A birefringent crystal;
example 18
Any of the NaVSeO obtained in examples 9-17 5 The birefringent crystal is used for preparing a wedge-shaped birefringent crystal polarization beam splitter (shown in fig. 4), the orientation of an optical axis is shown in fig. 4, a beam of natural light can be divided into two beams of linearly polarized light through the crystal after being incident, and the larger the birefringence, the farther the two beams of light can be separated, so that the separation of the beams of light is facilitated.
Example 19
Any of the NaVSeO obtained in examples 9-17 5 A crystal for preparing an optical isolator by placing a faraday rotator whose plane of polarization of an incident beam is rotated 45 ° between a pair of birefringent crystal deflectors disposed at 45 ° intersections with each other, can constitute an optical isolator that allows only forward propagating light beams to pass through the system while blocking backward propagating light beams, fig. 6a shows that the incident beam can pass through, and fig. 6b shows that the reflected light is blocked.
Example 20
Any of the NaVSeO obtained in examples 9-17 5 The crystal is used for preparing the light beam shifter, processing a birefringent crystal, and enabling the optical axis surface of the birefringent crystal to form an angle theta with the edge (shown in fig. 7 a), when natural light is vertically incident, the birefringent crystal can be divided into two linearly polarized lights (shown in fig. 7 b) with mutually perpendicular vibration directions, namely o light and e light, respectively, and the greater the double-fold rate is, the farther the two lights can be separated, so that the light beam separation is facilitated.
Claims (6)
1. A compound sodium vanadium selenite is characterized in that the chemical formula of the compound is NaVSeO 5 The molecular weight is 232.89, and the polymer is prepared by a vacuum packaging method.
2. The preparation method of the compound sodium vanadium selenite according to claim 1, which is characterized by adopting a vacuum packaging method, and comprises the following specific operations:
uniformly mixing Na-containing compound, V-containing compound and Se-containing compound according to the molar ratio of Na to V to Se=1:1:1, filling into quartz tube, and vacuum-pumping the quartz tube to vacuum degree of 10 -3 Pa, sealing at high temperature, placing in a muffle furnace,heating to 200-550deg.C at a rate of 5-10deg.C/h, and keeping the temperature for 24-100 hr to obtain NaVSeO 5 The Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 。
3. A sodium vanadium selenite birefringent crystal is characterized in that the chemical formula of the crystal is NaVSeO 5 The molecular weight is 232.89, the crystal belongs to monoclinic system and space groupC2/cThe unit cell parameters area=18.234(3)Å，b=3.8381(6)Å，c=12.416(2)Å，α=90°，β=112.421(7)°，γ=90°，V=803.2(2)Å 3 ，Z=8。
4. The method for preparing a sodium vanadium selenite birefringent crystal according to claim 3, wherein the crystal is grown by a sealed molten salt method, high Wen Rongye or vacuum encapsulation method, wherein:
the sealed molten salt growth NaVSeO 5 The birefringent crystal is prepared by the following steps:
a. uniformly mixing a Na-containing compound, a V-containing compound and a Se-containing compound according to the molar ratio of Na to V to Se=1 to 1, transferring into a lining of a high-pressure hydrothermal kettle, and sealing the high-pressure hydrothermal kettle, wherein the Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
b. Heating to 300-550deg.C at a rate of 5-10deg.C/h, maintaining the temperature for 2-3 days, slowly cooling to room temperature at a rate of 1-5deg.C/d, and opening the high pressure hydrothermal kettle to obtain NaVSeO 5 A birefringent crystal;
NaVSeO is prepared by the high-temperature melt method 5 The birefringent crystal is prepared by the following steps:
a. uniformly mixing Na-containing compound, V-containing compound and Se-containing compound according to the molar ratio of Na to V to Se=1 to 1, placing into a quartz tube, vacuumizing the quartz tube, and keeping the vacuum degree to 10 -3 Sealing at high temperature of Pa, placing in a muffle furnace, heating to 200-550deg.C at a speed of 5-10deg.C/h, and keeping constant temperature for 24-100 hr to obtain NaVSeO 5 The Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
b. Subjecting the compound NaVSeO obtained in step a to 5 Placing the mixture into a corundum crucible, heating to 450-600 ℃, and keeping the temperature for 5-100 hours to obtain mixed melt;
c. preparing seed crystals: c, placing the mixed solution obtained in the step b into a single crystal furnace, slowly cooling to 220 ℃ at the speed of 0.1-2 ℃/h, and rapidly cooling to room temperature at the speed of 5-10 ℃/h to obtain NaVSeO 5 Seed crystal;
d. growing a crystal: c, fixing the seed crystal obtained in the step c on a seed rod, applying 2-20rpm of crystal rotation from the upper side of the mixed solution obtained in the step b through a crystal growth controller, cooling at a speed of 0.1-3 ℃/h, and obtaining NaVSeO after the crystal growth is stopped 5 A birefringent crystal;
the vacuum packaging method prepares NaVSeO 5 The birefringent crystal is prepared by the following steps:
a. uniformly mixing Na-containing compound, V-containing compound and Se-containing compound according to the molar ratio of Na to V to Se=1 to 1, placing into a quartz tube, vacuumizing the quartz tube, and keeping the vacuum degree to 10 -3 Sealing at high temperature of Pa, placing in a muffle furnace, heating to 200-550deg.C at a speed of 5-10deg.C/h, and keeping constant temperature for 24-100 hr to obtain NaVSeO 5 The Na-containing compound is Na 2 CO 3 、Na 2 O、Na 2 SO 4 、NaNO 3 Or NaVO 3 The V-containing compound is V 2 O 5 Or NaVO 3 And the Se-containing compound SeO 2 Or H 2 SeO 4 ；
b. The NaVSeO obtained in the step a is treated 5 Placing the polycrystalline powder into a quartz tube, sealing at high temperature, placing into a muffle furnace, heating to 450-600deg.C, maintaining the temperature for 50-100 hr, cooling to 220deg.C at a rate of 0.1-3deg.C/h, and rapidly cooling to room temperature at a rate of 5-10deg.C/h to obtain NaVSeO 5 Birefringent crystals.
5. Use of a sodium vanadium selenite birefringent crystal according to claim 3 for the preparation of an optical communication element, namely an optical isolator, circulator, beam shifter, optical polarizer or optical modulator.
6. The method according to claim 5, wherein the use of the sodium vanadium selenite optical crystal in the manufacture of various polarizing prisms, i.e. phase retardation devices and electro-optical modulation devices.
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