Compound aminoguanidine monofluorophosphate monohydrate, birefringent crystal of aminoguanidine monofluorophosphate monohydrate, and preparation method and application of birefringent crystal of aminoguanidine monofluorophosphate monohydrate
By growing monohydrate aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O birefringent crystals using room temperature solution method and hydrothermal method, the shortcomings of existing materials in terms of large size and ease of processing are overcome, and the preparation of high-quality crystals and their application in optical components are realized.
Patent Information
- Application Number
- CN202610046790.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-14
- Publication Date
- 2026-03-03
AI Technical Summary
Existing birefringent crystal materials are insufficient in terms of overall performance, stability, and ease of large-size growth, making it difficult to meet the requirements of high-quality and large-size optical polarizing elements.
Birefringent crystals of aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O were grown using room temperature solution method and hydrothermal method. By controlling the crystal growth conditions and using a specific container liner, large-sized, transparent and easy-to-process crystals were obtained.
Large-sized, transparent, and easily processed (CN4H7)2PO3F·H2O birefringent crystals were obtained. The growth rate was fast and the cost was low, making them suitable for the fabrication of optical components such as optical isolators, circulators, beam shifters, and optical polarizers.
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Figure CN121591785A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a compound monohydrate aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O and a birefringent crystal of monohydrate aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O, as well as their preparation methods and uses. Background Technology
[0002] Birefringent optical crystals have significant applications in many fields, such as scientific research, transportation, national defense, and industry. With the exploration of birefringent crystal materials in recent years, a series of commercially viable birefringent materials have been discovered and developed. Examples include YVO4, LiNbO3, CaCO3, MgF2, and TiO2, whose applications cover the ultraviolet to infrared bands. However, these birefringent materials all have shortcomings: YVO4 is a high-performance artificial birefringent crystal, but due to its high melting point, it must be grown using an iridium crucible in a weak oxygen atmosphere, leading to iridium valence changes during growth and consequently reducing crystal quality, making it difficult to obtain high-quality crystals; LiNbO3 crystals are easy to obtain in large sizes, but its birefringence is too low; CaCO3, which mainly exists in natural form, is difficult to synthesize artificially, generally has small sizes, and high impurity content, failing to meet the requirements of large-size optical polarizing devices, and is also prone to dissociation, making processing difficult and resulting in low crystal utilization; MgF2's low birefringence also severely limits its widespread application; rutile TiO2 crystals have high hardness, making device processing and cutting difficult. Therefore, it is essential to find a birefringent crystal with a high birefringence, good and stable overall performance parameters, and ease of growing high-quality large-size bulk crystals.
[0003] Previous research has yielded three related patents: Ammonium monofluorophosphate nonlinear optical crystal and its preparation method and uses (patent application number CN201810212517.5), a class of nonlinear optical crystals, monofluorophosphate (patent application number CN201711475170.5), and a hydroxyphosphite aminoguanidine nonlinear optical crystal and its preparation method and uses (patent application number CN202410921095.4). The main difference between this invention and the above three patents is that the compound (CN4H7)2PO3F·H2O described in this invention has a space group of [space group missing]. P twenty one / c It belongs to the monoclinic crystal system. Furthermore, its growth habits, key growth process parameters, and linear optical properties differ from the previous three. Summary of the Invention
[0004] The purpose of this invention is to provide a compound, aminoguanidine monofluorophosphate monohydrate, with the chemical formula (CN4H7)2PO3F·H2O and a molecular weight of 266.20, prepared by a room temperature solution method.
[0005] Another object of the present invention is to provide a birefringent crystal of aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O, the chemical formula of which is (CN4H7)2PO3F·H2O, the molecular weight of which is 266.20, and the crystal structure belongs to the monoclinic crystal system with space group [missing information]. P twenty one / c The unit cell parameters are a = 4.9572(6) Å, b = 20.492(3) Å, c = 11.0338(16) Å, α =90°, β = 91.685(5)°, γ = 90°, unit cell volume is 1120.4(3) Å 3 .
[0006] Another objective of this invention is to provide a method for preparing a birefringent crystal of aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O, wherein the crystal is grown by hydrothermal method or room temperature solution method.
[0007] Another object of the present invention is to provide the use of a birefringent crystal of aminoguanidine monofluorophosphate (CN4H7)2PO3F·H2O.
[0008] The present invention discloses a compound, aminoguanidine monofluorophosphate monohydrate, with the chemical formula (CN4H7)2PO3F·H2O and a molecular weight of 266.20, which is prepared by room temperature solution method.
[0009] The compound aminoguanidine monofluorophosphate monohydrate is prepared by a room temperature solution method, and the specific operation is carried out according to the following steps: Mix the aminoguanidine compound and the PO3F compound at a molar ratio of 2:1 until homogeneous. Place the mixture in a clean container, add 20-100 mL of deionized water, and then sonicate to ensure thorough mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. Seal the container with plastic wrap, making several small holes in the seal, and let it stand for 5-20 days to obtain the compound (CN4H7)2PO3F·H2O. The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3, or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F.
[0010] A birefringent crystal of aminoguanidine monofluorophosphate monohydrate, with the chemical formula (CN4H7)2PO3F·H2O and a molecular weight of 266.20, belongs to the monoclinic crystal system and has a space group of [missing information]. P twenty one / c The unit cell parameters are a = 4.9572(6) Å, b = 20.492(3) Å, c = 11.0338(16) Å, α = 90°, β = 91.685(5)°, γ = 90°, unit cell volume is 1120.4(3)Å 3 .
[0011] The preparation method of the monohydrate aminoguanidine monofluorophosphate birefringent crystal involves growing the crystal using a hydrothermal method or a room temperature solution method. The hydrothermal growth of aminoguanidine monofluorophosphate birefringent crystal is carried out according to the following steps: a. Mix the aminoguanidine compound and the PO3F compound at a molar ratio of 2:1 until homogeneous, place in a container, add 30 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3 or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F. 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. c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 130-150 ℃ at a rate of 20-50℃ / h, keep the temperature constant for 5-8 days, and then lower the temperature to room temperature at a rate of 5-25 ℃ / day to obtain (CN4H7)2PO3F·H2O birefringent crystal. The room temperature solution method for growing aminoguanidine monofluorophosphate birefringent crystals is performed according to the following steps: a. Mix the aminoguanidine compound and the PO3F compound at a molar ratio of 2:1 until homogeneous, place the mixture in a clean container, add 20-100 mL of deionized water, and then sonicate to ensure thorough mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3, or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F. b. Place the mixed solution obtained in step a in a clean container, seal it with plastic wrap, 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 water in the aqueous solution. Let it stand for 5-20 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow for 10-30 days to obtain (CN4H7)2PO3F·H2O birefringent crystal.
[0012] The use of the monohydrated aminoguanidine monofluorophosphate birefringent crystal in the preparation of optical isolators, circulators, beam shifters, optical polarizers or optical modulators.
[0013] The optical polarizer is a polarizing beam splitter prism.
[0014] The polarizing beam splitter is a Glan prism, a Wollaston prism, or a Lochte prism.
[0015] The preparation method of the monohydrated aminoguanidine monofluorophosphate birefringent crystal of the present invention uses a plastic beaker as the container in the preparation process, and a hydrothermal reactor with a polytetrafluoroethylene liner or a stainless steel liner fitted with a platinum sleeve.
[0016] The method for preparing the birefringent crystal of aminoguanidine monofluorophosphate described in this invention uses a muffle furnace or a drying oven in the preparation process.
[0017] The preparation method of the monohydrate aminoguanidine monofluorophosphate birefringent crystal described in this invention can obtain large-sized (CN4H7)2PO3F·H2O birefringent crystals. By using a large-sized container and extending the crystal growth period, correspondingly large-sized (CN4H7)2PO3F·H2O crystals can be obtained. In the growth of this (CN4H7)2PO3F·H2O birefringent crystal, the crystal grows easily, is transparent and unencapsulated, and has the advantages of fast growth rate, low cost, and easy acquisition of large-sized crystals. Attached Figure Description
[0018] Figure 1 The powder XRD pattern of the compound (CN4H7)2PO3F·H2O of this invention; Figure 2 This is a structural diagram of the (CN4H7)2PO3F·H2O crystal of the present invention; Figure 3 The birefringence curve of the compound (CN4H7)2PO3F·H2O of this invention is shown. Figure 4This is a schematic diagram of the wedge-shaped birefringent crystal polarization 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 the (CN4H7)2PO3F·H2O crystal; Figure 5 This is a schematic diagram of the optical isolator of the present invention, where 6 represents the light transmission direction; 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
[0019] The present invention will be further described below with reference to embodiments. It should be noted that the following embodiments are not intended to limit the scope of protection of the present invention, and any improvements made based on the present invention do not depart from the spirit of the present invention. Unless otherwise specified, the raw materials or equipment used in the present invention are commercially available. Example 1
[0020] Based on the reaction equation: 2CN4H7Cl + H2PO3F + H2O → (CN4H7)2PO3F·H2O + 2HCl, the compound (CN4H7)2PO3F·H2O was synthesized using a room temperature solution method. Mix CN4H7Cl and H2PO3F at a molar ratio of 2:1 until homogeneous, place the mixture in a clean plastic beaker, add 20 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution, seal the beaker with plastic wrap, make several small holes in the seal, and let it stand for 5 days to obtain the compound (CN4H7)2PO3F·H2O. Example 2
[0021] Based on the reaction equation: 2CN4H7NO3 + H2PO3F + H2O → (CN4H7)2PO3F·H2O + 2HNO3, the compound (CN4H7)2PO3F·H2O was synthesized using a room temperature solution method. Mix CN4H7NO3 and H2PO3F at a molar ratio of 2:1 until homogeneous, place the mixture in a clean plastic beaker, add 40 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution, seal the beaker with plastic wrap, make several small holes in the seal, and let it stand for 15 days to obtain the compound (CN4H7)2PO3F·H2O. Example 3
[0022] Based on the reaction equation: 2CN4H6·H2CO3 + H2PO3F → (CN4H7)2PO3F·H2O + 2CO2 + H2O, the compound (CN4H7)2PO3F·H2O was synthesized using a room temperature solution method. Mix CN4H6·H2CO3 and H2PO3F in a molar ratio of 2:1 until homogeneous. Place the mixture in a clean plastic beaker, add 60 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. Seal the beaker with plastic wrap, making several small holes in the seal, and let it stand for 10 days to obtain the compound (CN4H7)2PO3F·H2O. Example 4
[0023] According to the reaction formula: (CN4H7)2SO4 + H2PO3F + H2O → (CN4H7)2PO3F·H2O + H2SO4, the compound (CN4H7)2PO3F·H2O was synthesized by a room temperature solution method. Mix (CN4H7)2SO4 and H2PO3F in a molar ratio of 1:1 until homogeneous. Place the mixture in a clean plastic beaker, add 80 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. Seal the beaker with plastic wrap, making several small holes in the seal, and let it stand for 20 days to obtain the compound (CN4H7)2PO3F·H2O. Example 5
[0024] Based on the reaction equation: 2CN4H7Cl + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + 2NaCl, the compound (CN4H7)2PO3F·H2O was synthesized using a room temperature solution method. Mix CN4H7Cl and Na2PO3F at a molar ratio of 2:1 until homogeneous, place the mixture in a clean plastic beaker, add 100 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution, seal the beaker with plastic wrap, make several small holes in the seal, and let it stand for 5 days to obtain the compound (CN4H7)2PO3F·H2O. Example 6
[0025] Based on the reaction equation: 2CN4H7NO3 + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + 2NaNO3, the compound (CN4H7)2PO3F·H2O was synthesized using a room temperature solution method. Mix CN4H7NO3 and Na2PO3F at a molar ratio of 2:1 until homogeneous, place the mixture in a clean plastic beaker, add 80 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution, seal the beaker with plastic wrap, make several small holes in the seal, and let it stand for 10 days to obtain the compound (CN4H7)2PO3F·H2O. Example 7
[0026] According to the reaction formula: (CN4H7)2SO4 + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + Na2SO4, the compound (CN4H7)2PO3F·H2O was synthesized by a room temperature solution method. Mix (CN4H7)2SO4 and Na2PO3F in a molar ratio of 1:1 until homogeneous. Place the mixture in a clean plastic beaker, add 60 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. Seal the beaker with plastic wrap, making several small holes in the seal, and let it stand for 15 days to obtain the compound (CN4H7)2PO3F·H2O. Example 8
[0027] Based on the reaction equation: 2CN4H7Cl + H2PO3F + H2O → (CN4H7)2PO3F·H2O + 2HCl, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix CN4H7Cl and H2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber and heat it to 130 ℃ at a rate of 20 ℃ / h. Hold the temperature for 5 days and then cool it down to room temperature at a rate of 5 ℃ / day. This will yield a (CN4H7)2PO3F·H2O birefringent crystal with dimensions of 6 mm × 3 mm × 1 mm. Example 9
[0028] Based on the reaction equation: 2CN4H7NO3 + H2PO3F + H2O → (CN4H7)2PO3F·H2O + 2HNO3, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix CN4H7NO3 and H2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber and heat it to 140 ℃ at a rate of 30 ℃ / h. Hold the temperature for 6 days and then cool it down to room temperature at a rate of 10 ℃ / day. This will yield a (CN4H7)2PO3F·H2O birefringent crystal with dimensions of 4 mm × 2 mm × 1 mm. Example 10
[0029] Based on the reaction equation: 2CN4H6·H2CO3 + H2PO3F → (CN4H7)2PO3F·H2O + 2CO2 + H2O, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix CN4H6·H2CO3 and H2PO3F evenly at a molar ratio of 2:1, put the mixture into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber and heat it to 145 ℃ at a rate of 40 ℃ / h. Hold the temperature for 7 days and then cool it down to room temperature at a rate of 15 ℃ / day. This will yield a (CN4H7)2PO3F·H2O birefringent crystal with dimensions of 4 mm × 4 mm × 1 mm. Example 11
[0030] Based on the reaction formula: (CN4H7)2SO4 + H2PO3F + H2O → (CN4H7)2PO3F·H2O + H2SO4, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix (CN4H7)2SO4 and H2PO3F evenly in a molar ratio of 1:1, put the mixture into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 150 ℃ at a rate of 50 ℃ / h, hold the temperature for 8 days, and then lower the temperature to room temperature at a rate of 20 ℃ / day to obtain a (CN4H7)2PO3F·H2O birefringent crystal with dimensions of 2 mm × 4 mm × 2 mm. Example 12
[0031] Based on the reaction equation: 2CN4H7Cl + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + 2NaCl, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix CN4H7Cl and Na2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 130 ℃ at a rate of 20 ℃ / h, hold the temperature for 8 days, and then lower the temperature to room temperature at a rate of 25 ℃ / day to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 4 mm × 5 mm × 1 mm. Example 13
[0032] Based on the reaction equation: 2CN4H7NO3 + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + 2NaNO3, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix CN4H7NO3 and Na2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber and heat it to 140 ℃ at a rate of 25 ℃ / h. Hold the temperature for 6 days and then cool it down to room temperature at a rate of 18 ℃ / day. This will yield a (CN4H7)2PO3F·H2O birefringent crystal with dimensions of 4 mm × 1 mm × 1 mm. Example 14
[0033] Based on the reaction formula: (CN4H7)2SO4 + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + Na2SO4, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using a hydrothermal method. a. Mix (CN4H7)2SO4 and Na2PO3F evenly in a molar ratio of 1:1, put the mixture into a plastic beaker, add 30 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. 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. c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 150 ℃ at a rate of 35 ℃ / h, hold the temperature for 7 days, and then lower the temperature to room temperature at a rate of 16 ℃ / day to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 5 mm × 2 mm × 1 mm. Example 15
[0034] Based on the reaction equation: 2CN4H7Cl + H2PO3F + H2O → (CN4H7)2PO3F·H2O + 2HCl, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using the room temperature solution method. a. Mix CN4H7Cl and H2PO3F evenly in a molar ratio of 2:1, put the mixture into a plastic beaker, add 20 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 5 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow for 10 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 3 mm × 2 mm × 1 mm. Example 16
[0035] Based on the reaction equation: 2CN4H7NO3 + H2PO3F + H2O → (CN4H7)2PO3F·H2O + 2HNO3, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using the room temperature solution method. a. Mix CN4H7NO3 and H2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 40 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 10 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 15 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 6 mm × 2 mm × 2 mm. Example 17
[0036] Based on the reaction equation: 2CN4H6·H2CO3 + H2PO3F → (CN4H7)2PO3F·H2O + 2CO2 + H2O, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using the room temperature solution method. a. Mix CN4H7NO3 and H2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 60 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 15 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 20 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 4 mm × 2 mm × 3 mm. Example 18
[0037] Based on the reaction equation: (CN4H7)2SO4 + H2PO3F + H2O → (CN4H7)2PO3F·H2O + H2SO4, birefringent crystals of (CN4H7)2PO3F·H2O were grown using the room temperature solution method. a. Mix (CN4H7)2SO4 and H2PO3F evenly in a molar ratio of 1:1, put the mixture into a plastic beaker, add 50 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 20 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 25 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 5 mm × 3 mm × 1 mm. Example 19
[0038] Based on the reaction equation: 2CN4H7Cl + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + 2NaCl, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using the room temperature solution method. a. Mix CN4H7Cl and Na2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 60 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 18 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 30 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 6 mm × 4 mm × 1 mm. Example 20
[0039] Based on the reaction equation: 2CN4H7NO3 + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + 2NaNO3, a birefringent crystal of (CN4H7)2PO3F·H2O was grown using the room temperature solution method. a. Mix CN4H7NO3 and Na2PO3F evenly at a molar ratio of 2:1, put them into a plastic beaker, add 80 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 16 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 26 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 5 mm × 1 mm × 2 mm. Example 21
[0040] Based on the reaction formula: (CN4H7)2SO4 + Na2PO3F + H2O → (CN4H7)2PO3F·H2O + Na2SO4, birefringent crystals of (CN4H7)2PO3F·H2O were grown using the room temperature solution method. a. Mix (CN4H7)2SO4 and Na2PO3F evenly in a molar ratio of 1:1, put them into a plastic beaker, add 100 mL of deionized water as a solvent, sonicate to fully mix and dissolve, and filter with filter paper to obtain a mixed solution. b. Place the mixed solution obtained in step a in a clean plastic beaker, seal it with plastic wrap, 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 water in the aqueous solution, and let it stand for 14 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 18 days to obtain a (CN4H7)2PO3F·H2O birefringent crystal with a size of 7 mm × 3 mm × 1 mm. Example 22
[0041] The arbitrary (CN4H7)2PO3F·H2O birefringent crystals obtained in Examples 8-21 were used to prepare 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 beam separation. Example 23
[0042] Using any of the (CN4H7)2PO3F·H2O birefringent crystals obtained in Examples 8-21 to prepare an optical isolator, a Faraday rotator with its incident beam polarization plane rotated by 45° is placed between a pair of birefringent crystal deflectors placed at 45° angles to each other, thus constructing an optical 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. Example 24
[0043] Any (CN4H7)2PO3F·H2O birefringent crystal obtained in Examples 8-21 is used to fabricate a beam shifter. 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 compound, aminoguanidine monofluorophosphate monohydrate, characterized in that... The compound has the chemical formula (CN4H7)2PO3F·H2O and a molecular weight of 266.
20. It was prepared by room temperature solution method.
2. A method for preparing the compound aminoguanidine monofluorophosphate as described in claim 1, characterized in that, The solution was prepared using a room temperature solution method, and the specific steps are as follows: Mix the aminoguanidine compound and the PO3F compound at a molar ratio of 2:1 until homogeneous. Place the mixture in a clean container, add 20-100 mL of deionized water, and then sonicate to ensure thorough mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. Seal the container with plastic wrap, making several small holes in the seal, and let it stand for 5-20 days to obtain the compound (CN4H7)2PO3F·H2O. The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3, or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F.
3. A birefringent crystal of aminoguanidine monofluorophosphate monohydrate, characterized in that, The crystal has the chemical formula (CN4H7)2PO3F·H2O, a molecular weight of 266.20, belongs to the monoclinic crystal system, and its space group is [space group number missing]. P twenty one / c The unit cell parameters are a = 4.9572(6)Å, b = 20.492(3) Å, c = 11.0338(16) Å, α = 90°, β = 91.685(5)°, γ = 90°, unit cell volume is 1120.4(3) Å 3 .
4. A method for preparing a birefringent crystal of aminoguanidine monofluorophosphate as described in claim 3, characterized in that, Crystals are grown using either hydrothermal or room temperature solution methods. The hydrothermal growth of aminoguanidine monofluorophosphate birefringent crystal is carried out according to the following steps: a. Mix the aminoguanidine compound and the PO3F compound at a molar ratio of 2:1 until homogeneous, place in a container, add 30 mL of deionized water as solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3 or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F. 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. c. Place the high-pressure reactor in a constant temperature chamber, raise the temperature to 130-150 ℃ at a rate of 20-50℃ / h, keep the temperature constant for 5-8 days, and then lower the temperature to room temperature at a rate of 5-25 ℃ / day to obtain (CN4H7)2PO3F·H2O birefringent crystal. The room temperature solution method for growing aminoguanidine monofluorophosphate birefringent crystals is performed according to the following steps: a. Mix the aminoguanidine compound and the PO3F compound at a molar ratio of 2:1 until homogeneous, place the mixture in a clean container, add 20-100 mL of deionized water, and then sonicate to ensure thorough mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3, or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F. b. Place the mixed solution obtained in step a in a clean container, seal it with plastic wrap, 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 water in the aqueous solution. Let it stand for 5-20 days. c. Wait for crystal particles to grow at the bottom of the container from the solution in step b, until the size of the crystal particles no longer changes significantly, and you will get a seed crystal. d. Select the seed crystal with better quality from step c, suspend it in the mixed solution prepared in step a, and let it grow statically for 10-30 days to obtain (CN4H7)2PO3F·H2O birefringent crystal.
5. The use of the monohydrate aminoguanidine monofluorophosphate birefringent crystal as described in claim 3 in the preparation of optical isolators, circulators, beam shifters, optical polarizers or optical modulators.
6. As described in claim 5, the optical polarizer is a polarizing beam splitter prism.
7. As described in claim 6, the polarizing beam splitter is a Glan prism, a Wollaston prism, or a Lochte prism.
Citation Information
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