NL2032981A - A Birefringent Crystal and Its Preparation Method - Google Patents

A Birefringent Crystal and Its Preparation Method Download PDF

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NL2032981A
NL2032981A NL2032981A NL2032981A NL2032981A NL 2032981 A NL2032981 A NL 2032981A NL 2032981 A NL2032981 A NL 2032981A NL 2032981 A NL2032981 A NL 2032981A NL 2032981 A NL2032981 A NL 2032981A
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birefringent
crystal
crystals
birefringent crystal
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NL2032981B1 (en
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Huang Ling
Zhang Die
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Univ Sichuan Normal
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/54—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
    • C30B7/04—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Polarising Elements (AREA)

Abstract

The invention discloses a birefringent crystal and its preparation method. The chemical formula of the birefringent crystal is [C(NH2)3]Sb(Czo4)F2(H20) or RbSb(CzO4)F2(H20), wherein [C(NH2)3]Sb(Czo4)F2(H20) can be prepared by deep eutectic solvents, solvent evaporation method or hydrothermal method, and RbSb(CzO4)F2(H20) can be prepared by hydrothermal reaction. The birefringent crystal prepared according to the invention has a birefringence index of 0165-0339 at 546nm, which is higher than that of the famous birefringent material or-BaBzO4. The crystal is colorless and transparent and has good chemical stability, which can expand the application range of linear optics in ultraviolet band.

Description

Sichuan Normal University 22/067 PDNL A Birefringent Crystal and Its Preparation Method Technical Field The invention belongs to the technical field of crystal material, in particular to a birefringent crystal and its preparation method thereof. Background Technology Birefringent materials have the function of modulating polarized light and play a key role in optical fiber sensors, advanced optical communication systems, linear and nonlinear optical devices, etc. One of the most important components of the polarizer is the birefringent crystal. When a beam of light is projected onto the crystal interface, two refraction beams will generally be generated. One of them follows the refraction law, which is called ordinary light or o-light, and the refractive index is constant. The other beam, which does not obey the law of refraction, is called extraordinary or e-light, and the refractive index varies depending on the direction the light travels, a phenomenon known as birefringence. Because the crystal material is anisotropic, the angle between the two refracted rays is related to the direction of propagation of the light wave and the state of polarization. The crystals that produce this birefringence are called birefringent crystals. As shown in Figure 1, when a beam of light is projected onto the calcite crystal interface, two refracted beams can be generated, with different propagation directions and velocities.
The birefringent crystal acts like a polarizer with two mutually perpendicular oscillating directions. At present, birefringent crystals have many uses in our practical life. For example, it can be used in various polarization devices, such as optical polarizers, beam splitters, wave plates, circulators and phase matching devices. In the past few decades, many kinds of birefringent materials have been synthesized and developed, including YVO,, TiO2, LINbO3, CaCO3, MgF: and a-BaB.O4(a-BBO) crystals. Among them, industrial calcite, YVO. and a-BaB:O, are widely used as polarizers and compensators. However, due to the limited application range of this kind of crystal, the design and synthesis of large birefringent materials are urgently needed, which is also the focus of current research.
Among the above birefringent materials, the most significant characteristic of simple binary halide MgF: is its ultra-wide transparent range (130nm-8um), which is the most commonly used deep ultraviolet birefringent material at present. However, due to its small birefringence (0.012@546nm), its practical application is severely limited. CaCO3 is the most common birefringent material in the commercial world and can be used in the visible or ultraviolet region. However, because it is a natural mineral and contains many impurities, it is difficult to make polarizing prism with high optical quality. YVO, crystal has a large birefringence, with a birefringence index of about 0.216 at 532nm. However, the crystal's wavelength below 400nm is opaque, and generally only applies to the near infrared range. Although a-BaB2O, crystals have good overall properties, their birefringence is smaller than that of YVO, and rutile, which impeds the miniaturization of optical elements and presents challenges to fabricating small optical elements.
Therefore, it is of great scientific and technological significance to invent a new type of ultraviolet birefringent crystal which is easy to grow single crystal, low cost, excellent performance and strong optical anisotropy for compact optical elements.
Description of the Invention The purpose of the invention is to provide a birefringent crystal and a preparation method thereof, which can solve the above problems.
To achieve the above purposes, the invention provides a birefringent crystal with chemical formula ASb(C.04)F2(H20), where A is Rb or C(NH:)a. The birefringent crystal has a birefringent index of 0.165-0.339 at 546nm.
Further, the chemical formula is [C{NH2)31Sb{C204)F2{H20) or RbSb{(C:O4)F2(H20). Specifically, the birefringency of [C{NHz)3]Sb{(C:04)F2{H20O) crystal at 546nm is 0.339, and that of RbSb{(C:O,4)F2(H2O) crystal at 546nm is 0.165.
Further, [C{NHz)3s]JSb(C:04)F2(H20) crystal is prepared from oxalic acid dihydrate, guanidine salt and antimony trifluoride with molar ratios of 1~2:1~2:2. Guanidine salts are guanidine carbonate or guanidine sulfate.
Furthermore, RbSb(C204)F2(H20) crystal preparation materials include oxalic acid dihydrate, rubidium salt and antimony trifluoride, the mole ratio of the three is 1~2:1~2:2; Rubidium salt is rubidium carbonate or RDF.
The preparation methods of birefringent crystals are hydrothermal reaction method, solvent evaporation method or deep eutectic solvents.
Hydrothermal reaction includes the following steps: (1) Add the formula amount of raw materials into deionized water and stir for 15- 25min; (2) The mixture was reacted at 80-90°C for 120-150h; (3) The reaction system is cooled to room temperature, single crystals are collected and washed to prepare birefringent crystals.
Further, the deep eutectic solvents method includes the following steps: (1) H2C204-H20 and SbF: were mixed and ground evenly in a certain proportion, and then placed in a polytetrafluoroethylene tube and placed in a constant temperature drying oven at 95~105°C to form a deep eutectic solvent. Then the mixture was added with guanidine salt and kept at the same temperature for 70~75h;
(2) The reaction system is cooled to room temperature, single crystals are collected and washed to prepare birefringent crystals.
Further, the solvent evaporation method includes the following steps: (1) Add the formula amount of raw materials into deionized water and stir for 15- 25min; (2) Filtrate the mixed solution, take the clear solution and volatile at 4-6 °C for 10- 15d; (3) Take out the volatilized product and wash it with deionized water to prepare the birefringent crystal. In conclusion, the invention has the following advantages:
1. In the present invention, oxalic acid, as an anionic group with planar TT conjugation, contributes greatly to the synthesis of crystals with large birefringence, and oxalic acid as a raw material can broaden the application of oxalic acid in the preparation of birefringent materials;
2. In the present invention, the Sb** cation with stereochemical activity lone pair electrons has a highly asymmetric structure and is a good birefringent active group; Rb* as a cation plays a role of charge compensation in the whole structure.
3. In the invention, the low-dimensional structure is more conducive to the superposition of linear optical birefringence. The introduction of F-atom can act as a chemical scissors to enable the compound to form low-dimensional chain structure, avoiding the formation of two-dimensional layer or even three-dimensional network structure, so as to effectively increase the birefringence of the compound.
4. In the present invention, [C(NH2)s]* has a planar triangular t-conjugated structure, which is conducive to increasing the total anisotropic polarization and thus increasing the birefringence of the compound.
5. The birefringence index of RbSb(C.04)F2(H20) prepared by the method provided by the invention is 0.165 at 546nm and the ultraviolet absorption edge is 321nm.
6. The birefringence index of [C{NHs)s]Sb(C2O4)F2(H20) prepared by the method provided by the invention is 0.339 at 546nm, and the ultraviolet absorption edge is 303nm.
7. The birefringent single crystal prepared by the method provided by the invention is colorless and transparent, has good chemical stability, is suitable for ultraviolet region, and can be used for linear optical applications in expanding ultraviolet band.
Brief Description of the Drawings Figure 1 is the birefringence phenomenon in calcite crystal; Figure 2 is the typical schematic diagram of RbSb(C204)F:(H20) or
[C(NH2)s]Sb(C204)F2(H20) crystals as birefringent crystals applied to polarizer; Among that, 1 is non-polarized light, 2 is polarizer, 3 is the glue part of two prisms made by RbSb(C204)F2(H20) or [C(NH2)s]Sb(C204)F2(H20) crystals after crystal processing and optical processing, 4 and 5 are two kinds of light beams with different refractive indexes, among which 4 is very light (e-light), 5 is ordinary light (o-light); Figure 3 is the X-ray diffraction pattern of RbSb(C.04)F2(H>0) single crystal after grinding into powder; Figure 4 is the X-ray diffraction pattern of RbSb(C.04)F2(H20) single crystal after grinding into powder and the diffraction pattern of computer fitting; Figure 5 is the birefringence results of RbSb(C.04)F2(H20) calculated by density functional method (DFT); Figure 6 is the schematic diagram of RbSb{(C204)F2(H2O) crystal structure; Figure 7 is the crystal structure of [C{NHz)3]Sb(C204)F2(H20); Figure 8 is the X-ray diffraction pattern of [C{NHz):]Sb(C204)F2(H20) single crystal after grinding into powder; Figure 9 is the X-ray diffraction pattern of [C(NH2)3]Sb(C204)F2(H20) single crystal after grinding into powder compared with the diffraction pattern fitted by computer; Figure 10 is the birefringence result of [C{NHz})3]Sb{C204)F2{H20) calculated by density Functional method (DFT).
Specific Implementation Methods The principles and characteristics of the invention are described in the following Implementation methods. The examples are only used to explain the invention, not to limit the scope of the invention. If the specific conditions are not specified in the embodiment, the general conditions or the conditions suggested by the manufacturer shall be followed. Reagents or instruments used without manufacturer indicated are conventional products that can be purchased through the market and are analytically pure. Implementation Method 1 This Implementation method provides a hydrothermal method for the synthesis of [C{NH:>)s]Sb(C:04)F2(H20) single crystal, including the following steps: (1) Weighing raw materials: 0.126g oxalic acid dihydrate, 0.090g guanidine carbonate, 0.179g antimony trifluoride and 3mL deionized water; (2) After mixing the raw material, put it into 23mL polytetrafluoroethylene liner, and then put it into stainless steel shell and tighten it, put it in a constant temperature drying oven at 85°C for 144h, then take it out of the drying oven, coal it at room temperature, and get Smmx2mmx 1mm colorless transparent single crystal;
(3) Birefringent crystal [C(NH2)3]Sb(C.04)F2(H20) is obtained after repeated washing with mother liquor and deionized water until the surface is free of impurities. Mother liquor is the liquid after single crystal precipitation.
5 Implementation Method 2 This Implementation method provides a deep eutectic solvents method for the synthesis of [C(NH2)s]Sb(C204)F2(H20) single crystal, including the following steps: (1) Weighing raw materials: 0.126g oxalic acid dihydrate, 0.180g guanidine carbonate, 0.1799 antimony trifluoride; (2) After mixing the raw materials in proportion and grinding them evenly with a mortar, they are put into a polytetrafluoroethylene tube and placed in a constant temperature drying oven at 100°C to form a deep eutectic solvent, and then reacted at the same temperature for 72h. Then they are removed from the drying oven and cooled at room temperature to obtain a colorless transparent single crystal of mm grade of 3mmx2mmx 1mm.
(3) Birefringent crystal [C(NH.)s]Sb(C204)F2(H20) is obtained by washing single crystal with anhydrous ethanol until the surface is free of impurities. Implementation Method 3 This Implementation method provides a hydrothermal reaction method for the synthesis of [C(NH2)3]Sb(C204)F2(H-0) single crystal, including the following steps: (1) Weighing raw materials: 0.126g oxalic acid dihydrate, 0.216g guanidine sulfate, 0.179g antimony trifluoride and 3mL deionized water; (2) After mixing the raw materials, put them into 23mL polytetrafluoroethylene liner, and then put them into the stainless steel shell and tighten them, put them into the constant temperature drying oven at 85°C for 120h, then take them out of the drying oven and cool them at room temperature to obtain colorless transparent single crystal of 4mmx1.5mmx0.5mm; (3) Birefringent crystal [C(NH2)3]Sb(C.04)F2(H20) is obtained after repeated washing of single crystal with mother liquor and deionized water until the surface is free of impurities. Mother liquor is the liquid after single crystal precipitation.
Implementation Method 4 This Implementation method provides a solvent evaporation method for the synthesis of [C(NHz)3]Sb(C204)F2(H2O) single crystal, including the following steps: (1) Weighing raw materials: 0.1269 oxalic acid dihydrate, 0.180g guanidine carbonate and 0.358g antimony trifluoride;
(2) After mixing the raw materials, add 5mL deionized water and stir to dissolve it. Strain the undissolved material with a quick filter paper and pour the liquid into a plastic beaker. Then itis placed in a refrigerator at 5°C for 10-15 days, and then removed from the refrigerator to obtain a colorless transparent single crystal of 4mmx3mmx0.5mm; (3) Birefringent crystal [C(NH2)3]Sb(C204)F2(H2zO) is obtained after the single crystal is washed with deionized water until the surface is free of impurities. Implementation Method 5 This Implementation method provides a solvent evaporation method for the synthesis of [C{NH2):]Sb(C204)F2(H20) single crystal, including the following steps: (1) Weighing raw materials: 0.063g oxalic acid dihydrate, 0.218g guanidine sulfate and 0.179g antimony trifluoride; (2) After mixing the raw materials in proportion, add 5mL deionized water and stir to dissolve it. Strain the undissolved material with a quick filter paper and pour the liquid into a plastic beaker. And then put it in the refrigerator at 5°C, about 15 days from the refrigerator, 5Smmx1mmx 0.5mm colorless transparent single crystal; (3) After the single crystal is washed with deionized water to the surface without impurities, the birefringent crystal-antimony guanidine fluoride oxalate hydrate is obtained.
Implementation Method 8 This Implementation method provides a hydrothermal reaction method for the synthesis of RbSb(C,04)F2(H20) single crystal, including the following steps: (1) Weighing raw materials: 0.252g oxalic acid dihydrate, 0.231g rubidium carbonate and 0.358g antimony trifluoride; (2) Mix the raw materials in proportion, add 3mL deionized water and mix them evenly, put them into 23mL polytetrafluoroethylene inner liner, then put them into stainless steel shell and tighten them, put them in a constant temperature drying oven at 85°C for 120- 144h, then take them out of the drying oven and cool them at room temperature. The colorless transparent single crystal of 4mmx1.5mmx0.5mm is obtained.
(3) Birefringent crystal RbSb(C.04)F2(H20) is obtained after repeated washing with mother liquor and anhydrous ethanol until the surface is free of impurities. Mother liquor is the liquid after single crystal precipitation.
The monocellular structure of crystal [C(NH2):]Sb(C204)F2(H.0) prepared in implementation method 1 is shown in Figure 7. After grinding the single crystal, the powder is tested by X-ray diffraction test. The X-ray diffraction pattern is shown in Figure 8 and compared with the pattern simulated by computer, as shown in Figure 9. The experimental result is consistent with the simulated result of X-ray single crystal diffraction, indicating that the powder sample is pure phase. The birefringence of [C(NH:):]Sb(C204)F2(H20) is calculated using density functional method (DFT). The birefringence of [C(NH2)3]Sb(C204)F2(H>0) at 546nm is about 0.339 (Figure 10 in the attached drawings), which is larger than any commercially available birefringent material. [C{NH2)3]Sb(C204)F:(H2O) single crystal is colorless and transparent and has good chemical stability. In addition, its ultraviolet absorption edge is 303nm. It can be predicted that [C(NH2)3]Sb(C204)F2(H-0) will find applications in birefringent materials and open up linear optical applications in the ultraviolet band.
The monocellular structure of RbSb(C:O4)F2(H20) crystal prepared in implementation method 6 is shown in Figure 6. The birefringency of RbSb(C2O4)F2(H20O) is calculated using density functional method (DFT). The birefringency of RbSb(C2O4)F2(H20) at 546nm is about 0.165 (as shown in Figure 5), which is larger than the famous birefringent oa-BaB:O4 (0.122@546nm). Its ultraviolet absorption edge is 321nm. In addition, RbSb(C20O4)F2(H20) single crystal is colorless and transparent, and has good chemical stability.
After grinding the single crystal, X-ray diffraction test is conducted on the powder. The XRD pattern is shown in Figure 3 and compared with the pattern simulated by computer, as shown in Figure 4. Comparison result show that the experimental patterns are consistent with the simulated results of X-ray single crystal diffraction, indicating that the powder sample is pure phase.
Although the specific implementation methods of the present invention are described in detail, they should not be understood as limiting the scope of protection of the present patent. In the scope described in the claim, the technical personnel in this field can make all kinds of modification and deformation without creative labor still belong to the scope of protection of this patent.

Claims (8)

ConclusiesConclusions 1. Dubbelbrekend kristal, met het kenmerk, dat het kristal de chemische formule ASb(C204)F2(H20) heeft, waarbij A Rb of C(NH2)sis, en een dubbelbrekingsindex heeft vanA birefringent crystal, characterized in that the crystal has the chemical formula ASb(C204)F2(H2O), wherein A is Rb or C(NH2)sis, and has a birefringence index of 0.165-0.339 bij 546nm.0.165-0.339 at 546nm. 2. Dubbelbrekend kristal volgens conclusie 1, met het kenmerk, dat de chemische formule [C(NH2)3]Sb(C204)F:(H20) of RbSb(C.04)F2(H20) is, en de dubbelbrekingsindex van [C(NHz)3]Sb(C204)F2(H20) en RbSb(C20.)F2(H20) kristallen bij 546nm respectievelijkThe birefringent crystal according to claim 1, characterized in that the chemical formula is [C(NH2)3]Sb(C204)F:(H2O) or RbSb(C04)F2(H2O), and the birefringence index of [ C(NHz)3]Sb(C204)F2(H2O) and RbSb(C20.)F2(H2O) crystals at 546nm respectively 0.339 en 0.165 is.0.339 and 0.165. 3. Dubbelbrekend kristal volgens conclusie 2, met het kenmerk, dat de grondstoffen voor de bereiding van [C(NH2)3]Sb(C204)F2(H20) kristallen oxaalzuurdihydraat, guanidinezout en antimoontrifluoride omvatten, waarbij de molaire verhouding van deze drie stoffen 1-2: 1-2: 2 is, waarbij het guanidinezout guanidinecarbonaat of guanidinesulfaat is.The birefringent crystal according to claim 2, characterized in that the raw materials for the preparation of [C(NH2)3]Sb(C2O4)F2(H2O) crystals comprise oxalic acid dihydrate, guanidine salt and antimony trifluoride, the molar ratio of these three substances 1-2:1-2:2, wherein the guanidine salt is guanidine carbonate or guanidine sulfate. 4. Dubbelbrekend kristal volgens conclusie 2, met het kenmerk, dat de grondstoffen voor de bereiding van RbSb(C:04)F:(H2O) kristallen oxaalzuurdihydraat, rubidiumzout en antimoontrifluoride omvatten, waarbij de molaire verhouding van deze drie stoffen 1-2 : 1-2 : 2 is, waarbij het rubidiumzout rubidiumcarbonaat of RDF is.The birefringent crystal according to claim 2, characterized in that the raw materials for the preparation of RbSb(C:04)F:(H2O) crystals comprise oxalic acid dihydrate, rubidium salt and antimony trifluoride, the molar ratio of these three substances being 1-2: 1-2 : 2, wherein the rubidium salt is rubidium carbonate or RDF. 5. Werkwijze voor de bereiding van een dubbelbrekend kristal, zoals gedefinieerd in éen van de conclusies 1-4, met het kenmerk, dat de werkwijze een hydrothermische reactiemethode, een oplosmiddelverdampingsmethode of een diep eutectische oplos- middelmethode omvat.A method for preparing a birefringent crystal as defined in any one of claims 1-4, characterized in that the method comprises a hydrothermal reaction method, a solvent evaporation method or a deep eutectic solvent method. 6. Werkwijze volgens conclusie 5, met het kenmerk, dat de hydrothermische reactiemethode uit de volgende stappen bestaat: (1) Voeg de hoeveelheid grondstoffen volgens de formule toe aan gedeminerali- seerd water en roer gedurende 15-25min; (2) Laat het mengsel gedurende 120-150 uur reageren bij 80-90°C; (3) Koel het reactiesysteem af tot kamertemperatuur, verzamel de enkelvoudige kristallen en was deze om dubbelbrekende kristallen te bereiden.A method according to claim 5, characterized in that the hydrothermal reaction method consists of the following steps: (1) Add the amount of raw materials according to the formula to demineralized water and stir for 15-25 min; (2) Allow the mixture to react at 80-90°C for 120-150 hours; (3) Cool the reaction system to room temperature, collect the single crystals and wash them to prepare birefringent crystals. 7. Werkwijze volgens conclusie 5, met het kenmerk, dat de diep eutectische oplosmiddelmethode uit de volgende stappen bestaat:Method according to claim 5, characterized in that the deep eutectic solvent method consists of the following steps: (1) Meng H2C:04H20 en SbF; en maal dit gelijkmatig fijn in een bepaalde verhouding, en plaats het mengsel vervolgens in een buis van polytetrafluorethyleen in een droogoven met constante temperatuur bij 95-105°C om een diep eutectisch oplosmiddel te vormen; (2) Voeg guanidinezout aan het mengsel toe en houd dit gedurende 70-75 uur op dezelfde temperatuur; (3) Koel het reactiesysteem af tot kamertemperatuur, verzamel de enkelvoudige kristallen en was deze om dubbelbrekende kristallen te bereiden.(1) Mix H2C:04H2O and SbF; and grind it evenly in a certain proportion, and then place the mixture in a polytetrafluoroethylene tube in a constant temperature drying oven at 95-105°C to form a deep eutectic solvent; (2) Add guanidine salt to the mixture and keep it at the same temperature for 70-75 hours; (3) Cool the reaction system to room temperature, collect the single crystals and wash them to prepare birefringent crystals. 8. Werkwijze volgens conclusie 5, met het kenmerk, dat de oplosmiddel- verdampingsmethode uit de volgende stappen bestaat: (1) Voeg de hoeveelheid grondstoffen volgens de formule toe aan gedeminerali- seerd water en roer gedurende 15-25min; (2) Filtreer de gemengde oplossing, neem de heldere oplossing en laat deze gedurende 10-15 dagen vervluchtigen bij 4-6°C; (3) Isoleer het vervluchtigde product en was het met gedemineraliseerd water om het dubbelbrekende kristal te bereiden.The method according to claim 5, characterized in that the solvent evaporation method consists of the following steps: (1) Add the amount of raw materials according to the formula to demineralized water and stir for 15-25 min; (2) Filter the mixed solution, take the clear solution and volatilize it at 4-6°C for 10-15 days; (3) Isolate the volatilized product and wash it with deionized water to prepare the birefringent crystal.
NL2032981A 2021-12-27 2022-09-07 A Birefringent Crystal and Its Preparation Method NL2032981B1 (en)

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