Compound potassium fluoroiodoborate and potassium fluoroiodoborate birefringent crystal and preparation method and use

Potassium fluoroiodate birefringent crystals were prepared by hydrothermal method or room temperature solution method, which solved the problem of insufficient existing ultraviolet birefringent materials and obtained large-size transparent crystals suitable for optical equipment.

CN118164436BActive Publication Date: 2026-06-19XINJIANG TECH INST OF PHYSICS & CHEM CHINESE ACAD OF SCI

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
XINJIANG TECH INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
Filing Date
2024-03-13
Publication Date
2026-06-19

Smart Images

  • Figure CN118164436B_ABST
    Figure CN118164436B_ABST
Patent Text Reader

Abstract

This invention relates to a compound potassium fluoroiodate and a linear birefringent optical crystal of potassium fluoroiodate, as well as their preparation methods and uses. The chemical formula of the compound is KI4O. 10 F, with a molecular weight of 725.70, was prepared by hydrothermal or room temperature solution methods. This compound belongs to the triclinic crystal system, space group P1(_), with cell parameters a=7.1685(3) Å, b=7.4967(3) Å, and c=10.9225(4) Å. α =102.823(1)°, β =90.704(1)°, gamma =114.431(1)°, Z =2, V=517.50(4)Å 3 The crystal is grown using a hydrothermal method or a room-temperature solution method. It has a low ultraviolet cutoff edge and a large birefringence of 0.133@1064nm. Its excellent performance and good chemical stability make it suitable for fabricating polarizing prisms, phase delay devices, and electro-optic modulation devices for various applications, such as Glan prisms, polarization beam splitters, compensators, optical isolators, circulators, and optical modulators. It plays an important role in the fields of optics and communications.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to a compound potassium fluoroiodate and a potassium fluoroiodate birefringent crystal, as well as their preparation methods and uses. Background Technology

[0002] Polarized light is a fascinating phenomenon in nature, leading to numerous discoveries and applications. Birefringent materials are among the key materials for realizing polarized light and are widely used in optical devices that generate polarized light, such as polarizers for modern laser applications, optical isolators, and prism polarizers. To date, some birefringent materials, such as MgF2, CaCO3, α-BaB2O4, and YVO4, have been used in the ultraviolet (UV), visible, and infrared regions. However, these birefringent crystals still cannot meet the needs of practical industry and scientific research. Therefore, there is an urgent need to explore new high-quality ultraviolet birefringent material systems and novel superior ultraviolet birefringent material systems and superior functional groups with better performance to meet these challenges. Summary of the Invention

[0003] The purpose of this invention is to provide a compound, potassium fluoroiodate, with the chemical formula KI4O. 10 F, with a molecular weight of 725.70, is prepared by hydrothermal method or room temperature solution method.

[0004] Another object of the present invention is to provide a potassium fluoroiodate birefringent optical crystal with the chemical formula KI4O. 10 F, molecule

[0005] The crystal density is 725.70, belonging to the triclinic system, and the space group is [missing information]. Cell parameters are α=102.823(1)°, β=90.704(1)°, γ=114.431(1)°, Z=2,

[0006] Another objective of this invention is to provide a method for preparing potassium fluoroiodate birefringent crystals, using a hydrothermal method or a room temperature solution method.

[0007] Another object of the present invention is to provide the use of potassium fluoroiodate birefringent crystals.

[0008] The present invention discloses a compound, potassium fluoroiodate, with the chemical formula KI4O. 10 F, with a molecular weight of 725.70, is prepared by hydrothermal method or room temperature solution method.

[0009] The compound potassium fluoroiodate is prepared by a hydrothermal method or a room temperature solution method, and the specific operation is carried out according to the following steps:

[0010] The compound potassium fluoroiodate is prepared using a hydrothermal method.

[0011] a. Mix the K-containing compound, I-containing compound, and F-containing compound in a molar ratio of 1:4:1 until homogeneous, add 0.5-5 mL of deionized water to fully mix and dissolve, and obtain a mixed solution; wherein the K-containing compound is K2CO3, KHCO3, KF, or KIO3, the I-containing compound is HIO3, I2O5, or KIO3, and the F-containing compound is KF, HF, or KHF2;

[0012] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0013] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 180-230℃ at a rate of 20-50℃ / h, maintain the temperature for 2-5 days, then lower the temperature to room temperature at a rate of 1-10℃ / h. Open the high-temperature reactor to obtain compound KI4O. 10 F;

[0014] The compound potassium fluoroiodate is prepared using a room temperature solution method.

[0015] a. Mix the K-containing compound, I-containing compound, and F-containing compound evenly in a molar ratio of 1:4:1, place them in a polytetrafluoroethylene beaker, add 5-20 mL of deionized water, and stir to fully mix and dissolve the compounds. The K-containing compound is K2CO3, KHCO3, KF, or KIO3, the I-containing compound is HIO3, I2O5, or KIO3, and the F-containing compound is KF, HF, or KHF2.

[0016] b. Seal the container containing the solution from step a with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain compound KI4O. 10 F.

[0017] A potassium fluoroiodate birefringent crystal with the chemical formula KI4O 10 F, with a molecular weight of 725.70, belongs to the triclinic crystal system.

[0018] Space group is Cell parameters are α=102.823(1)°, β=90.704(1)°, γ=114.431(1)°, Z=2,

[0019] The preparation method of the sodium fluoroborate nonlinear optical crystal adopts a hydrothermal method or a room temperature solution method to grow the crystal;

[0020] The hydrothermal growth of potassium fluoroiodate birefringent crystals is carried out according to the following steps:

[0021] a. Mix the K-containing compound, I-containing compound, and F-containing compound in a molar ratio of 1:4:1 until homogeneous, add 5-30 mL of deionized water to fully mix and dissolve, and obtain a mixed solution; wherein the K-containing compound is K2CO3, KHCO3, KF, or KIO3, the I-containing compound is HIO3, I2O5, or KIO3, and the F-containing compound is KF, HF, or KHF2;

[0022] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated high-pressure reactor with a volume of 23-100 mL, and tighten and seal the reactor.

[0023] c. Place the high-pressure reactor in a constant temperature chamber and heat it to 180-230℃ at a rate of 20-50℃ / h. Maintain the temperature for 2-5 days, and then cool it down to room temperature at a rate of 1-3℃ / h. Open the high-pressure reactor and obtain large-sized potassium fluoroiodate birefringent crystals in the millimeter size from the colorless clear solution.

[0024] The potassium fluoroiodate birefringent crystal was grown using a room temperature solution method.

[0025] a. Mix the K-containing compound, I-containing compound, and F-containing compound evenly in a molar ratio of 1:4:1, place them in a polytetrafluoroethylene beaker, add 20-100 mL of deionized water, and stir to fully mix and dissolve the compounds. The K-containing compound is K2CO3, KHCO3, KF, or KIO3, the I-containing compound is HIO3, I2O5, or KIO3, and the F-containing compound is KF, HF, or KHF2.

[0026] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment without shaking, pollution, or air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate in the solution. The growth is then complete, and a potassium fluoroiodate birefringent crystal with a size in the millimeter range is obtained.

[0027] The potassium fluoroiodate birefringent crystal is used in the fabrication of optical isolators, circulators, beam shifters, optical polarizers, or optical modulators.

[0028] The optical polarizer is a polarizing beam splitter prism.

[0029] The polarizing beam splitter is a Glan prism, a Wollaston prism, or a Lochte prism.

[0030] The method for preparing potassium fluoroiodate birefringent crystals according to the present invention uses conical flasks, polytetrafluoroethylene beakers, plastic beakers, or hydrothermal reactors with polytetrafluoroethylene linings or stainless steel linings fitted with platinum sleeves as containers. When the container is a conical flask, polytetrafluoroethylene beaker, or other similar container, it must first be cleaned with acid, then rinsed with deionized water, and then dried.

[0031] The method for preparing potassium fluoroborate nonlinear optical crystals described in this invention requires a muffle furnace or a drying oven as the resistance furnace used in the preparation process.

[0032] The method for preparing potassium fluoroiodate birefringent crystals described in this invention yields KI4O. 10 F-type birefringent crystals do not exhibit a distinct layered growth habit. By using a large-sized container and extending the crystal growth period, correspondingly large-sized birefringent crystals KI4O can be obtained. 10 F, in the KI4O 10 F-type birefringent crystals are easy to grow into transparent, unencapsulated crystals, and have advantages such as fast growth rate, low cost, and easy acquisition of large-size crystals. Attached Figure Description

[0033] Figure 1 The present invention KI4O 10 Powder XRD pattern of F;

[0034] Figure 2 The present invention KI4O 10 Structural diagram of F crystal;

[0035] Figure 3 The present invention KI4O 10 Birefringence curve of F crystal;

[0036] Figure 4 This is a schematic diagram of the wedge-shaped birefringent crystal polarizing beam splitter of the present invention, where 1 is the incident light, 2 is the o-ray, 3 is the e-ray, 4 is the optical axis, and 5 is KI4O. 10 F crystal;

[0037] Figure 5 This is a schematic diagram of the optical isolator of the present invention, where 6 represents the light transmission direction;

[0038] Figure 6 This is a schematic diagram of the beam shifter of the present invention, where 2 is the o-beam, 3 is the e-beam, 4 is the optical axis, and 7 is the optical axis plane. Detailed Implementation

[0039] The present invention will be further described below with reference to the embodiments. It should be noted that the embodiments are not intended to limit the scope of protection of the present invention. Unless otherwise specified, the raw materials or equipment used in the present invention are commercially available.

[0040] Example 1

[0041] Preparation of compounds:

[0042] According to the reaction formula: KF + 2I₂O₅ → KI₄O 10 F, Preparation of compound KI4O by hydrothermal method 10 F:

[0043] a. Mix KF and I2O5 evenly at a molar ratio of 1:2, add 0.5 mL of deionized water to mix and dissolve them thoroughly to obtain a mixed solution;

[0044] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0045] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 230℃ at a rate of 20℃ / h, maintain the temperature for 5 days, then lower it to room temperature at a rate of 5℃ / h. Open the high-temperature reactor to obtain compound KI4O. 10 F.

[0046] Example 2

[0047] Preparation of compounds:

[0048] According to the reaction formula: KF + 4HIO3 → KI4O 10 F + 2H₂O, compound KI₄O was prepared by a hydrothermal method. 10 F:

[0049] a. Mix KF and HIO3 evenly at a molar ratio of 1:4, add 1 mL of deionized water to mix and dissolve thoroughly to obtain a mixed solution;

[0050] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0051] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 220°C at a rate of 30°C / h, maintain the temperature for 4 days, then lower the temperature to room temperature at a rate of 10°C / h. Open the high-temperature reactor to obtain KI4O. 10 F compound.

[0052] Example 3

[0053] Preparation of compounds:

[0054] According to the reaction formula: KIO3 + 3HIO3 + HF → KI4O 10 F + 2H₂O, compound KI₄O was prepared by a hydrothermal method. 10 F:

[0055] a. Mix KIO3, HIO3 and HF in a molar ratio of 1:3:1 until homogeneous, add 5 mL of deionized water and mix thoroughly to obtain a mixed solution;

[0056] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0057] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 180°C at a rate of 30°C / h, maintain the temperature for 2 days, then lower the temperature to room temperature at a rate of 1°C / h. Open the high-temperature reactor to obtain KI4O. 10 F compound.

[0058] Example 4

[0059] Preparation of compounds:

[0060] According to the reaction formula: KHCO3 + 4HIO3 + HF → KI4O 10 F + 3H₂O + CO₂, compound KI₄O is prepared by a hydrothermal method. 10 F:

[0061] a. Mix KHCO3, HIO3 and HF evenly in a molar ratio of 1:4:1, add 3 mL of deionized water to mix and dissolve thoroughly to obtain a mixed solution;

[0062] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0063] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 190℃ at a rate of 20℃ / h, maintain the temperature for 3 days, then lower it to room temperature at a rate of 4℃ / h. Open the high-temperature reactor to obtain KI4O. 10 F compound.

[0064] Example 5

[0065] Preparation of compounds:

[0066] According to the reaction equation: K₂CO₃ + 8HIO₃ + 2HF → 2KI₄O 10 The compound KI4O is prepared by a hydrothermal method using the reaction F + 5H2O + 2CO2. 10 F:

[0067] a. Mix K2CO3, HIO3 and HF evenly in a molar ratio of 1:8:2, add 4 mL of deionized water to mix and dissolve thoroughly to obtain a mixed solution;

[0068] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0069] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 210℃ at a rate of 20℃ / h, maintain the temperature for 2 days, then lower it to room temperature at a rate of 3℃ / h. Open the high-temperature reactor to obtain KI4O. 10 F compound.

[0070] Example 6

[0071] Preparation of compounds:

[0072] According to the reaction formula: KOH + 4HIO3 + HF → KI4O 10 F + 3H₂O, compound KI₄O is prepared by hydrothermal method. 10 F:

[0073] a. Mix KOH, HIO3 and HF in a molar ratio of 1:4:1 until homogeneous, add 5 mL of deionized water and mix thoroughly to obtain a mixed solution;

[0074] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0075] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 230°C at a rate of 25°C / h, maintain the temperature for 3 days, then lower it to room temperature at a rate of 6°C / h. Open the high-temperature reactor to obtain KI4O. 10 F compound.

[0076] Example 7

[0077] Preparation of compounds:

[0078] According to the reaction formula: KOH + 8HIO3 + KHF2 → KI4O 10 F + 5H₂O, compound KI₄O is prepared by hydrothermal method. 10 F:

[0079] a. Mix KOH, HIO3 and KHF2 in a molar ratio of 1:8:1 until homogeneous, add 3 mL of deionized water and mix thoroughly to obtain a mixed solution;

[0080] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0081] c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 230℃ at a rate of 50℃ / h, maintain the temperature for 4 days, then lower it to room temperature at a rate of 7℃ / h. Open the high-temperature reactor to obtain KI4O. 10 F crystal.

[0082] Example 8

[0083] Preparation of compounds:

[0084] According to the reaction formula: KF + 4HIO3 → KI4O 10 F + 2H₂O, compound KI₄O was prepared by a room temperature solution method. 10 F:

[0085] a. Mix KF and HIO3 evenly at a molar ratio of 1:4, put them into a polytetrafluoroethylene beaker, add 5 mL of deionized water, and stir to make the compound fully mixed and dissolved;

[0086] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain the compound KI4O. 10 F.

[0087] Example 9

[0088] Preparation of compounds:

[0089] According to the reaction formula: KF + 2I₂O₅ → KI₄O 10 F, Preparation of compound KI4O by room temperature solution method 10 F:

[0090] a. Mix KF and I2O5 evenly in a 1:2 ratio, put them into a polytetrafluoroethylene beaker, add 20mL of deionized water, and stir to make the compound fully mixed and dissolved;

[0091] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain the compound KI4O. 10 F.

[0092] Example 10

[0093] Preparation of compounds:

[0094] According to the reaction formula: KOH + 2I₂O₅ + HF → KI₄O 10 F, Preparation of compound KI4O by room temperature solution method 10 F:

[0095] a. Mix KOH, I2O5 and HF evenly in a molar ratio of 1:2:1, put them into a polytetrafluoroethylene beaker, add 20mL of deionized water, and stir to make the compound fully mixed and dissolved.

[0096] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain the compound KI4O. 10 F.

[0097] Example 11

[0098] Preparation of compounds:

[0099] According to the reaction formula: KIO3 + 3HIO3 + HF → KI4O 10 F + 2H₂O, compound KI₄O was prepared by a room temperature solution method. 10 F:

[0100] a. Mix KIO3, HIO3 and HF evenly in a molar ratio of 1:3:1, put them into a polytetrafluoroethylene beaker, add 10 mL of deionized water, and stir to make the compound fully mixed and dissolved.

[0101] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain the compound KI4O. 10 F.

[0102] Example 12

[0103] Preparation of compounds:

[0104] According to the reaction equation: K₂CO₃ + 4HIO₃ + 2HF → 2KI₄O 10 F + 3H₂O + CO₂, compound KI₄O is prepared by a room temperature solution method. 10 F:

[0105] a. Mix K2CO3, HIO3 and HF evenly in a molar ratio of 1:4:2, put them into a polytetrafluoroethylene beaker, add 15mL of deionized water, and stir to make the compound fully mixed and dissolved.

[0106] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain the compound KI4O. 10 F.

[0107] Example 13

[0108] Preparation of compounds:

[0109] According to the reaction formula: KHCO3 + 8HIO3 + KHF2 → 2KI4O 10 The compound KI4O is prepared by a room-temperature solution method using the reaction F + 5H2O + CO2. 10 F:

[0110] a. Mix K2CO3, HIO3, and KHF2 evenly in a molar ratio of 1:8:1, place the mixture in a polytetrafluoroethylene beaker, add 20 mL of deionized water, and stir to ensure the compound is fully mixed and dissolved.

[0111] b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment free from shaking, contamination, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate from the solution, indicating the growth is complete. Quickly wash the product in the polytetrafluoroethylene beaker with deionized water and air dry at room temperature to obtain the compound KI4O. 10 F.

[0112] Example 14

[0113] According to the chemical reaction equation: KF + 2I₂O₅ → KI₄O 10 F, KI4O was grown using a hydrothermal method. 10 F-birefringent crystal:

[0114] a. Mix KF and I2O5 evenly at a molar ratio of 1:2, add 15mL of deionized water to mix and dissolve thoroughly to obtain a mixed solution;

[0115] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 50 mL high-pressure reactor, and tighten and seal the reactor.

[0116] c. The high-pressure reactor was placed in a constant temperature chamber and heated to 230℃ at a rate of 30℃ / h. The temperature was maintained for 4 days, and then cooled to room temperature at a rate of 1℃ / h. The high-pressure reactor was opened, and potassium fluoroiodate birefringent crystals with diameters of Φ1mm×0.7mm×0.5mm were obtained from the colorless clear solution.

[0117] Example 15

[0118] According to the chemical reaction equation: KF + 4HIO3 → KI4O 10 F + 2H₂O, KI₄O grown using a hydrothermal method 10 F-birefringent crystal:

[0119] a. Mix KF and HIO3 evenly at a molar ratio of 1:4, add 5 mL of deionized water to mix and dissolve thoroughly to obtain a mixed solution;

[0120] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 23 mL high-pressure reactor, and tighten and seal the reactor.

[0121] c. Place the high-pressure reactor in a constant temperature chamber and heat it to 220℃ at a rate of 25℃ / h. Maintain the temperature for 5 days, then cool it down to room temperature at a rate of 2℃ / h. Open the high-pressure reactor and obtain Φ0.9mm×0.6mm×0.5mm potassium fluoroiodate birefringent crystals from the colorless clear solution.

[0122] Example 16

[0123] According to the chemical reaction equation: KIO3 + 3HIO3 + HF → KI4O 10 F + 2H₂O, KI₄O grown using a hydrothermal method 10 F-birefringent crystal:

[0124] a. Mix KIO3, HIO3, and HF in a molar ratio of 1:3:1 until homogeneous, add 30 mL of deionized water and mix thoroughly to obtain a mixed solution;

[0125] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 100 mL high-pressure reactor and tighten and seal the reactor.

[0126] c. Place the high-pressure reactor in a constant temperature chamber and heat it to 210℃ at a rate of 50℃ / h. Maintain the temperature for 2 days, and then cool it down to room temperature at a rate of 1℃ / h. Open the high-pressure reactor and obtain a Φ1.5mm×1.1mm×0.7mm potassium fluoroiodate birefringent crystal from the colorless clear solution.

[0127] Example 17

[0128] According to the chemical reaction equation: KHCO3 + 4HIO3 + HF → KI4O 10 F + 3H₂O + CO₂, KI₄O is grown using a hydrothermal method. 10 F-birefringent crystal:

[0129] a. Mix KHCO3, HIO3 and HF evenly in a molar ratio of 1:4:1, add 30 mL of deionized water to mix and dissolve thoroughly to obtain a mixed solution;

[0130] b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated 100 mL high-pressure reactor and tighten and seal the reactor.

[0131] c. Place the high-pressure reactor in a constant temperature chamber and heat it to 180℃ at a rate of 20℃ / h. Maintain the temperature for 4 days, and then cool it down to room temperature at a rate of 1℃ / h. Open the high-pressure reactor and obtain a Φ1.8mm×1.3mm×0.8mm potassium fluoroiodate birefringent crystal from the colorless clear solution.

[0132] Example 18

[0133] According to the chemical reaction equation: KIO3 + 3HIO3 + HF → KI4O 10 F + 2H₂O, KI₄O₂ grown using room temperature solution method 10 F-birefringent crystal:

[0134] a. Mix KIO3, HIO3 and HF evenly in a molar ratio of 1:3:1, put them into a polytetrafluoroethylene beaker, add 100mL of deionized water, and stir to make the compound fully mixed and dissolved.

[0135] b. Seal the polytetrafluoroethylene beaker containing the solution from step a with a polyvinyl chloride film, and place it in a static environment free from shaking, pollution, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate in the solution. The growth is then complete, and a potassium fluoroiodate birefringent crystal with a diameter of 1.5 mm × 1.2 mm × 0.9 mm is obtained.

[0136] Example 19

[0137] According to the chemical reaction equation: KOH + 8HIO3 + KHF2 → 2KI4O 10 F+5H2O, KI4O is grown using the room temperature solution method. 10 F-birefringent crystal:

[0138] a. Mix KOH, HIO3 and KHF2 evenly in a molar ratio of 1:8:1, put them into a polytetrafluoroethylene beaker, add 50 mL of deionized water, and stir to make the compound fully mixed and dissolved.

[0139] b. Seal the polytetrafluoroethylene beaker containing the solution from step a with a polyvinyl chloride film, and place it in a static environment free from shaking, pollution, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate in the solution. The growth is then complete, and a potassium fluoroiodate birefringent crystal with a diameter of Φ1mm×0.7mm×0.6mm is obtained.

[0140] Example 20

[0141] According to the chemical reaction equation: KOH + 4HIO3 + HF → KI4O 10 F + 3H₂O was used to grow KI₄O using a room temperature solution method. 10 F-birefringent crystal:

[0142] a. Mix KOH, HIO3, and HF evenly in a molar ratio of 1:4:1, place the mixture in a polytetrafluoroethylene beaker, add 20 mL of deionized water, and stir to ensure the compound is fully mixed and dissolved.

[0143] b. Seal the polytetrafluoroethylene beaker containing the solution from step a with a polyvinyl chloride film, and place it in a static environment free from shaking, pollution, and air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate in the solution. The growth is then complete, and a potassium fluoroiodate birefringent crystal with a diameter of 0.7 mm × 0.5 mm × 0.4 mm is obtained.

[0144] Example 21

[0145] Any KI4O obtained in Examples 14-20 10 F-type birefringent crystals are used to fabricate wedge-shaped birefringent crystal polarization beam splitters (such as...). Figure 4 As shown), a wedge-shaped birefringent crystal, with its optical axis oriented as follows. Figure 4 As shown, a beam of natural light can be split into two linearly polarized beams after passing through a crystal. The greater the birefringence, the farther the two beams can be separated, which facilitates the separation of the beams.

[0146] Example 22

[0147] Any KI4O obtained in Examples 14-20 10 F-type birefringent crystals are used to fabricate optical isolators. An optical isolator is constructed by placing a Faraday rotator (with its incident beam polarization plane rotated by 45°) between a pair of birefringent crystal deflectors placed at 45° angles to each other. This creates an isolator that allows only forward-propagating beams to pass through the system while blocking backward-propagating beams. Figure 5 'a' indicates that the incident light beam can pass through. Figure 5 b indicates that the reflected light is blocked.

[0148] Example 23

[0149] Any KI4O obtained in Examples 14-20 10 F-type birefringent crystals are used to fabricate beam shifters. A birefringent crystal is fabricated such that its optical axis plane forms an angle θ with the edge (e.g., ...). Figure 6 As shown in a), when natural light is incident perpendicularly, it can be split into two beams of linearly polarized light with mutually perpendicular vibration directions (as shown in a). Figure 6 (As shown in b), these are the o-ray and e-ray, respectively. The greater the birefringence, the farther the two beams can be separated, which facilitates beam separation.

Claims

1. A potassium fluoroiodate birefringent crystal, characterized in that... The chemical formula of this crystal is KI4O 10 F, with a molecular weight of 725.70, belongs to the triclinic crystal system and has a space group of [missing information]. The unit cell parameters are a = 7.1685(3) Å, b = 7.4967(3) Å, c = 10.9225(4) Å, α = 102.823(1)°, β = 90.704(1)°, γ = 114.431(1)°, Z = 2, V = 517.50(4) Å. 3 .

2. A method for preparing potassium fluoroiodate birefringent crystal as described in claim 1, characterized in that... Crystals are grown using either hydrothermal or room-temperature solution methods. The hydrothermal growth of potassium fluoroiodate birefringent crystals is carried out according to the following steps: a. Mix the K-containing compound, I-containing compound, and F-containing compound in a molar ratio of 1:4:1 until homogeneous, add 5-30 mL of deionized water to fully mix and dissolve, and obtain a mixed solution; wherein the K-containing compound is K2CO3, KHCO3, KF, or KIO3, the I-containing compound is HIO3, I2O5, or KIO3, and the F-containing compound is KF, HF, or KHF2; b. Transfer the mixed solution obtained in step a into the liner of a clean, uncontaminated high-pressure reactor with a volume of 23-100 mL, and tighten and seal the reactor. c. Place the high-pressure reactor in a constant temperature chamber and heat it to 180-230℃ at a rate of 20-50℃ / h. Maintain the temperature for 2-5 days, and then cool it down to room temperature at a rate of 1-3℃ / h. Open the high-pressure reactor and obtain large-sized potassium fluoroiodate birefringent crystals in the millimeter size from the colorless clear solution. The potassium fluoroiodate birefringent crystal was grown using a room temperature solution method. a. Mix the K-containing compound, I-containing compound, and F-containing compound evenly in a molar ratio of 1:4:1, place them in a polytetrafluoroethylene beaker, add 20-100 mL of deionized water, and stir to fully mix and dissolve the compounds. The K-containing compound is K2CO3, KHCO3, KF, or KIO3, the I-containing compound is HIO3, I2O5, or KIO3, and the F-containing compound is KF, HF, or KHF2. b. Seal the polytetrafluoroethylene beaker containing the solution with a polyvinyl chloride film and place it in a static environment without shaking, pollution, or air convection. Make several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Let it stand at room temperature until crystals gradually precipitate in the solution. The growth is then complete, and a potassium fluoroiodate birefringent crystal with a size in the millimeter range is obtained.

3. The use of the potassium fluoroiodate birefringent crystal as described in claim 1 in the preparation of optical isolators, circulators, beam shifters, optical polarizers or optical modulators.

4. The use as described in claim 3, wherein the optical polarizer is a polarizing beam splitter prism.

5. The use as described in claim 4, wherein the polarizing beam splitter is a Glan prism, a Wollaston prism, or a Lochte prism.