Compound N-(isopropylimido) guanidine monofluorophosphate monohydrate and N-(isopropylimido) guanidine monofluorophosphate monohydrate birefringent crystal as well as preparation method and application of N-(isopropylimido) guanidine monofluorophosphate monohydrate birefringent crystal
By growing birefringent crystals of the compound monohydrated N-(isopropylimino)guanidine monofluorophosphate (C4N4H11)2PO3F·H2O, the problem of insufficient performance of existing materials in the ultraviolet, visible and infrared regions is solved, and high-quality birefringent materials are provided for optical devices.
Patent Information
- Application Number
- CN202610046840.4
- 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 materials cannot meet the needs of industrial and scientific research in the ultraviolet, visible and infrared regions, and there is a lack of high-quality birefringent material systems and functional groups with excellent performance.
Birefringent crystals of compound monohydrate N-(isopropylimino)guanidine monofluorophosphate (C4N4H11)2PO3F·H2O were grown using room temperature solution method and hydrothermal method. Large-sized transparent crystals were obtained by controlling the crystal growth parameters. The preparation was carried out in a hydrothermal reactor with a polytetrafluoroethylene liner or a platinum sleeve.
Large-sized, transparent, unencapsulated birefringent crystals were obtained with fast growth speed and low cost, making them suitable for optical devices such as polarizers, optical isolators, and beam shifters, achieving better optical performance.
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Figure CN121591786A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a compound, monohydrated N-(isopropylimino)guanidine monofluorophosphate (C4N4H 11 )2PO3F·H2O and monohydrated N-(isopropylimino)guanidine monofluorophosphate (C4N4H 11 Birefringent crystal of 2PO3F·H2O, its preparation method 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 and CaCO3, have been used to develop polarized light. α Materials such as BaB₂O₄ and YVO₄ have been used in the ultraviolet, 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 birefringent material systems and novel high-quality ultraviolet birefringent material systems and dominant functional groups with better performance to meet these challenges.
[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 (C4N4H) described in this invention... 11 )2PO3F·H2O, space group is It belongs to the triclinic crystal system. Furthermore, its growth habit, 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, N-(isopropylimino)guanidine monofluorophosphate monohydrate, with the chemical formula (C4N4H). 11 )2PO3F·H2O, with a molecular weight of 346.32, was prepared by room temperature solution method.
[0005] Another object of the present invention is to provide a hydrated N-(isopropylimino)guanidine monofluorophosphate (C4N4H 11 )2PO3F·H2O birefringent crystal, the chemical formula of which is (C4N4H11 2PO3F·H2O has a molecular weight of 346.32. Its crystal structure belongs to the triclinic system, and its space group is [space group number missing]. The unit cell parameters are a = 7.3372(6) Å, b = 9.0541(8) Å, c = 12.6489(10) Å, α = 96.383(3)°, β = 96.496(3)°, γ = 97.670(3)°, unit cell volume is 820.59(12) Å 3 .
[0006] Another object of the present invention is to provide monohydrated N-(isopropylimino)guanidine monofluorophosphate (C4N4H 11 The preparation method of 2PO3F·H2O birefringent crystals involves growing crystals using either a hydrothermal method or a room temperature solution method.
[0007] Another object of the present invention is to provide monohydrated N-(isopropylimino)guanidine monofluorophosphate (C4N4H 11 Applications of 2PO3F·H2O birefringent crystals.
[0008] The present invention discloses a compound, N-(isopropylimino)guanidine monofluorophosphate monohydrate, the chemical formula of which is (C4N4H). 11 )2PO3F·H2O, with a molecular weight of 346.32, was prepared by room temperature solution method.
[0009] The preparation method of the compound monohydrated N-(isopropylimino)guanidine monofluorophosphate is carried out by room temperature solution method, and the specific operation is as follows: Mix the aminoguanidine compound, the PO3F compound, and acetone in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, add 20-100 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 container with plastic wrap, making several small holes in the seal, and let it stand for 5-20 days to obtain the compound (C4N4H). 11 The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3 or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F.
[0010] A birefringent crystal of N-(isopropylimino)guanidine monofluorophosphate monohydrate, the chemical formula of which is (C4N4H 112PO3F·H2O, with a molecular weight of 346.32, belongs to the triclinic crystal system and has a space group of The unit cell parameters are a = 7.3372(6) Å, b = 9.0541(8) Å, c = 12.6489(10) Å, α = 96.383(3)°, β = 96.496(3)°, γ =97.670(3)°, unit cell volume is 820.59(12) Å 3 .
[0011] The preparation method of the monohydrated N-(isopropylimino)guanidine monofluorophosphate involves growing crystals using a hydrothermal method or a room temperature solution method. The hydrothermal growth of monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystals is carried out according to the following steps: a. Mix the aminoguanidine compound, the PO3F compound, and acetone in a molar ratio of 2:1:2 until homogeneous, place the mixture in a container, add deionized water as a solvent, and 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. 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 100-120℃ at a rate of 20-50℃ / h, maintain the temperature for 5-10 days, and then lower it to room temperature at a rate of 5-25℃ / day to obtain (C4N4H). 11 )2PO3F·H2O birefringent crystal; The room temperature solution method for growing monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystals is performed according to the following steps: a. Mix the aminoguanidine compound, the PO3F compound, and acetone in a molar ratio of 2:1:2 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.
[0012] 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 high-quality seed crystals from step c, suspend them in the mixed solution prepared in step a, and allow them to grow statically for 10-30 days to obtain (C4N4H). 11 )2PO3F·H2O birefringent crystal.
[0013] The use of the monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystal in the preparation of optical isolators, circulators, beam shifters, optical polarizers or optical modulators.
[0014] The optical polarizer is a polarizing beam splitter prism.
[0015] The polarizing beam splitter is a Glan prism, a Wollaston prism, or a Lochte prism.
[0016] The method for preparing monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystals of the present invention uses a hydrothermal autoclave with a polytetrafluoroethylene liner or a stainless steel liner fitted with a platinum sleeve during the preparation process; and a muffle furnace or a drying oven is used as the resistance furnace.
[0017] The method for preparing monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystals described in this invention yields large-sized (C4N4H) crystals. 11 By using a large-sized container and extending the crystal growth period, a birefringent crystal (C₄N₄H₂O) can be obtained, resulting in a correspondingly large-sized crystal. 11 )2PO3F·H2O, in the (C4N4H 11 The growth of 2PO3F·H2O birefringent crystals is characterized by easy growth, transparency, and no encapsulation. It has advantages such as fast growth rate, low cost, and easy acquisition of large-size crystals. Attached Figure Description
[0018] Figure 1 The compound of this invention (C4N4H) 11 Powder XRD pattern of 2PO3F·H2O; Figure 2 This invention (C4N4H) 11 Structural diagram of 2PO3F·H2O crystal; Figure 3 The compound of this invention (C4N4H) 11Birefringence curve of 2PO3F·H2O; 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 (C4N4H) 11 )2PO3F·H2O crystals; 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] According to the reaction equation: 2CN4H7Cl + H2PO3F + 2C3H6O → (C4N4H 11 The compound (C4N4H) was synthesized by a room-temperature solution method using the reaction 2PO3F·H2O + H2O + 2HCl. 11 )2PO3F·H2O: Mix CN4H7Cl, H2PO3F, and C3H6O in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 5 days to obtain compound (C4N4H). 11 )2PO3F·H2O. Example 2
[0021] According to the reaction equation: 2CN4H7NO3 + H2PO3F + 2C3H6O → (C4N4H 11 The compound (C4N4H) was synthesized by a room-temperature solution method using the reaction 2PO3F·H2O + 2HNO3 + H2O. 11 )2PO3F·H2O: Mix CN4H7NO3, H2PO3F, and C3H6O in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 15 days to obtain compound (C4N4H). 11)2PO3F·H2O. Example 3
[0022] According to the reaction equation: 2CN4H6·H2CO3 + H2PO3F + 2C3H6O → (C4N4H 11 The compound (C4N4H) was synthesized by a room-temperature solution method using the reaction 2PO3F·H2O + 2CO2 + 3H2O. 11 )2PO3F·H2O: Mix CN4H6·H2CO3, H2PO3F, and C3H6O in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 10 days to obtain the compound (C4N4H). 11 )2PO3F·H2O. Example 4
[0023] According to the reaction formula: (CN4H7)2SO4 + H2PO3F + 2C3H6O → (CN4H7)2PO3F·H2O + H2O + H2SO4, compound (C4N4H) was synthesized by room temperature solution method. 11 )2PO3F·H2O: Mix (CN4H7)2SO4, H2PO3F, and C3H6O in a molar ratio of 1:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 20 days to obtain the compound (C4N4H). 11 )2PO3F·H2O. Example 5
[0024] According to the reaction formula: 2CN4H7Cl + Na2PO3F + 2C3H6O → (C4N4H 11 The compound (C4N4H) was synthesized by a room-temperature solution method using the reaction 2PO3F·H2O + 2NaCl + H2O. 11 )2PO3F·H2O: Mix CN4H7Cl, Na2PO3F, and C3H6O in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 5 days to obtain compound (C4N4H). 11 )2PO3F·H2O. Example 6
[0025] According to the reaction equation: 2CN4H7NO3 + Na2PO3F + 2C3H6O → (C4N4H 11 The compound (C4N4H) was synthesized by a room-temperature solution method using the reaction 2PO3F·H2O + 2NaNO3 + H2O. 11 )2PO3F·H2O: Mix CN4H7NO3, Na2PO3F, and C3H6O in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 10 days to obtain compound (C4N4H). 11 )2PO3F·H2O. Example 7
[0026] According to the reaction formula: (CN4H7)2SO4 + Na2PO3F + 2C3H6O → (C4N4H 11 The compound (C4N4H) was synthesized by a room-temperature solution method using the reaction 2PO3F·H2O + Na2SO4 + H2O. 11 )2PO3F·H2O: Mix (CN4H7)2SO4, Na2PO3F, and C3H6O in a molar ratio of 1:1:2 until homogeneous. Place the mixture in a clean container, 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 container with plastic wrap, making several small holes in the seal, and let it stand for 15 days to obtain compound (C4N4H). 11 )2PO3F·H2O. Example 8
[0027] According to the reaction equation: 2CN4H7Cl + H2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + H2O + 2HCl, grown using a hydrothermal method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7Cl, H2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into 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. 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 100℃ at a rate of 20℃ / h, maintain the temperature for 5 days, and then lower it to room temperature at a rate of 5℃ / day. This yields (C4N4H) with dimensions of 6 mm × 3 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 9
[0028] According to the reaction equation: 2CN4H7NO3 + H2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2HNO3 + H2O, grown using a hydrothermal method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7NO3, H2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into 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. 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 105℃ at a rate of 30℃ / h, maintain the temperature for 6 days, and then lower it to room temperature at a rate of 10℃ / day. This yields (C4N4H) with dimensions of 4 mm × 2 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 10
[0029] According to the reaction equation: 2CN4H6·H2CO3 + H2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2CO2 + 3H2O, grown using a hydrothermal method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H6·H2CO3, H2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into 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. 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 110℃ at a rate of 40℃ / h, maintain the temperature for 7 days, and then lower it to room temperature at a rate of 15℃ / day. This yields (C4N4H) atoms with dimensions of 4 mm × 4 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 11
[0030] According to the reaction formula: (CN4H7)2SO4 + H2PO3F + 2C3H6O → (CN4H7)2PO3F·H2O + H2O + H2SO4, (C4N4H)2SO4 is grown using a hydrothermal method. 11 )2PO3F·H2O birefringent crystal: a. Mix (CN4H7)2SO4, H2PO3F, and C3H6O evenly in a molar ratio of 1:1:2, put the mixture into 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. 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 115℃ at a rate of 50℃ / h, maintain the temperature for 8 days, and then lower it to room temperature at a rate of 20℃ / day. This yields (C4N4H) atoms with dimensions of 2 mm × 4 mm × 2 mm. 11 )2PO3F·H2O birefringent crystal. Example 12
[0031] According to the reaction formula: 2CN4H7Cl + Na2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2NaCl + H2O, grown using a hydrothermal method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7Cl, Na2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into 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. 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 120℃ at a rate of 20℃ / h, maintain the temperature for 9 days, and then lower it to room temperature at a rate of 25℃ / day. This yields (C4N4H) particles with dimensions of 4 mm × 5 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 13
[0032] According to the reaction equation: 2CN4H7NO3 + Na2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2NaNO3 + H2O, grown using a hydrothermal method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7NO3, Na2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into 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. 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 110℃ at a rate of 25℃ / h, hold the temperature for 10 days, and then lower it to room temperature at a rate of 18℃ / day. This yields (C4N4H) particles with dimensions of 4 mm × 1 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 14
[0033] According to the reaction formula: (CN4H7)2SO4 + Na2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + Na2SO4+H2O, grown using a hydrothermal method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix (CN4H7)2SO4, Na2PO3F, and C3H6O evenly in a molar ratio of 1:1:2, put the mixture into a container, add 30mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, 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 100℃ at a rate of 35℃ / h, maintain the temperature for 7 days, and then lower it to room temperature at a rate of 16℃ / day. This yields (C4N4H) with dimensions of 5 mm × 2 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 15
[0034] According to the reaction equation: 2CN4H7Cl + H2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + H2O + 2HCl, grown using room temperature solution method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7Cl, H2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into a container, add 20 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 10 days to obtain a (C4N4H) crystal with dimensions of 3 mm × 2 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 16
[0035] According to the reaction formula 2CN4H7NO3 + H2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2HNO3 + H2O, using room temperature solution method to grow (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7NO3, H2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into a container, add 40 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 15 days to obtain a (C4N4H) crystal with dimensions of 6 mm × 2 mm × 2 mm. 11 )2PO3F·H2O birefringent crystal. Example 17
[0036] According to the reaction equation: 2CN4H6·H2CO3 + H2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2CO2 + 3H2O, grown using room temperature solution method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H6·H2CO3, H2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into a container, add 60 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 20 days to obtain a (C4N4H) crystal with dimensions of 4 mm × 2 mm × 3 mm. 11 )2PO3F·H2O birefringent crystal. Example 18
[0037] According to the reaction formula: (CN4H7)2SO4 + H2PO3F + 2C3H6O → (CN4H7)2PO3F·H2O + H2O + H2SO4, (C4N4H)2SO4 was grown using the room temperature solution method. 11 )2PO3F·H2O birefringent crystal: a. Mix (CN4H7)2SO4, H2PO3F, and C3H6O evenly in a molar ratio of 1:1:2, put the mixture into a container, add 50 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 25 days to obtain a (C4N4H) crystal with dimensions of 5 mm × 3 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 19
[0038] According to the reaction formula: 2CN4H7Cl + Na2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2NaCl + H2O, using room temperature solution method to grow (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7Cl, Na2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into a container, add 60 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 30 days to obtain a (C4N4H) crystal with dimensions of 6 mm × 4 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 20
[0039] According to the reaction equation: 2CN4H7NO3 + Na2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + 2NaNO3 + H2O, using room temperature solution method to grow (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix CN4H7NO3, Na2PO3F, and C3H6O evenly in a molar ratio of 2:1:2, put the mixture into a container, add 80 mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 26 days to obtain a (C4N4H) crystal with dimensions of 5 mm × 1 mm × 2 mm. 11 )2PO3F·H2O birefringent crystal. Example 21
[0040] According to the reaction formula: (CN4H7)2SO4 + Na2PO3F + 2C3H6O → (C4N4H 11 )2PO3F·H2O + Na2SO4 + H2O, grown using room temperature solution method (C4N4H 11 )2PO3F·H2O birefringent crystal: a. Mix (CN4H7)2SO4, Na2PO3F, and C3H6O evenly in a molar ratio of 1:1:2, put the mixture into a container, add 100mL of deionized water as a solvent, sonicate to ensure thorough mixing and dissolution, and filter with filter paper to obtain a mixed solution. 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, 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 high-quality seed crystal from step c, suspend it in the mixed solution prepared in step a, and allow it to grow statically for 18 days to obtain a (C4N4H) crystal with dimensions of 7 mm × 3 mm × 1 mm. 11 )2PO3F·H2O birefringent crystal. Example 22
[0041] Any (C4N4H) obtained in Examples 8-21 11 )2PO3F·H2O birefringent crystal, 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 the separation of the beams. Example 23
[0042] Any (C4N4H) obtained in Examples 8-21 11 A 2PO3F·H2O birefringent crystal is 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 isolator 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 (C4N4H) obtained in Examples 8-21 11 )2PO3F·H2O birefringent crystal, 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 compound, N-(isopropylimino)guanidine monofluorophosphate monohydrate, characterized in that, The chemical formula of this compound is (C4N4H). 11 )2PO3F·H2O, with a molecular weight of 346.32, was prepared by room temperature solution method.
2. A method for preparing the compound monohydrated N-(isopropylimino)guanidine 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, the PO3F compound, and acetone in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, add 20-100 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 container with plastic wrap, making several small holes in the seal, and let it stand for 5-20 days to obtain the compound (C4N4H). 11 The aminoguanidine compound is CN4H7Cl, CN4H7NO3, CN4H6·H2CO3 or (CN4H7)2SO4; the PO3F compound is H2PO3F or Na2PO3F.
3. A birefringent crystal of N-(isopropylimino)guanidine monofluorophosphate monofluorophosphate monohydrate, characterized in that, The chemical formula of this crystal is (C4N4H). 11 2PO3F·H2O, with a molecular weight of 346.32, belongs to the triclinic crystal system and has a space group of The unit cell parameters are a =7.3372(6) Å, b = 9.0541(8) Å, c = 12.6489(10) Å, α = 96.383(3)°, β = 96.496(3)°, γ = 97.670(3)°, unit cell volume is 820.59(12) Å 3 .
4. A method for preparing N-(isopropylimino)guanidine monofluorophosphate as described in claim 3, characterized in that... Crystals are grown using either hydrothermal or room temperature solution methods. The hydrothermal growth of monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystals is carried out according to the following steps: a. Mix the aminoguanidine compound, the PO3F compound, and acetone in a molar ratio of 2:1:2 until homogeneous, place the mixture in a container, add deionized water as a solvent, and 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. 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 100-120℃ at a rate of 20-50℃ / h, maintain the temperature for 5-10 days, and then lower it to room temperature at a rate of 5-25℃ / day to obtain (C4N4H). 11 )2PO3F·H2O birefringent crystal; The room temperature solution method for growing monohydrated N-(isopropylimino)guanidine monofluorophosphate birefringent crystals is performed according to the following steps: a. Mix the aminoguanidine compound, the PO3F compound, and acetone in a molar ratio of 2:1:2 until homogeneous. Place the mixture in a clean container, add 20-100 mL of deionized water, and then sonicate to ensure complete mixing and dissolution. Filter the mixture through filter paper to obtain a mixed solution. 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 high-quality seed crystals from step c, suspend them in the mixed solution prepared in step a, and allow them to grow statically for 10-30 days to obtain (C4N4H). 11 )2PO3F·H2O birefringent crystal.
5. The use of the monohydrated N-(isopropylimino)guanidine 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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