Compound diglycine trifluoromethanesulfonate and diglycine trifluoromethanesulfonate nonlinear optical crystal, and preparation method and application of compound diglycine trifluoromethanesulfonate and diglycine trifluoromethanesulfonate nonlinear optical crystal

Abstract

The invention relates to a compound diglycine trifluoromethane sulfonate and a diglycine trifluoromethane sulfonate nonlinear optical crystal as well as a preparation method and an application of the compound diglycine trifluoromethane sulfonate nonlinear optical crystal. The chemical formula of the compound diglycine trifluoromethane sulfonate is (C4N2O4H11) (CF3SO3), the molecular weight is 268.144, the chemical formula of the crystal is (C4N2O4H11) (CF3SO3), the crystal belongs to a monoclinic system, the space group is Cc, the cell parameters are a = 14.8353 (5), b = 8.9818 (3), c = 10.0267 (4), alpha = gamma = 90 degrees, beta = 120.090 (1) degrees, Z = 4, and the unit cell volume is 1155.99 (7) 3, and a room temperature solution method, a solvothermal method and a water bath heating method are adopted for preparation. The crystal shows excellent optical properties, including ideal birefringence, relatively short ultraviolet absorption edge of about 216 nm and moderate frequency-doubled effect of about one time of KH2PO4 (KDP). The crystal is easy to grow, does not deliquesce in air, has good chemical stability, and can be used as an ultraviolet nonlinear optical crystal in an all-solid-state laser.

Description

Technical Field

[0001] This invention relates to a compound, diglycine trifluoromethanesulfonate, and a nonlinear optical crystal of diglycine trifluoromethanesulfonate, as well as their preparation methods and uses. Background Art

[0002] Nonlinear optical (NLO) crystals play a crucial role in frequency conversion in solid-state lasers. Over the past few decades, researchers have discovered a series of NLO crystals, such as β-BaB₂O₄ (β-BBO), LiNbO₃, and KH₂PO₄ (KDP). However, to meet the demands of laser science and technology development, the continued development of novel NLO crystals—especially those suitable for the short-wavelength ultraviolet (UV) region—remains essential. From a structural design perspective, ideal short-wavelength UV NLO candidates should meet the following requirements: 1) possessing a non-centrosymmetric structure; 2) having a short UV absorption cutoff wavelength (λ). cutoff 3) Large second harmonic response (≥ 1 × KDP); 4) Suitable birefringence (Δn = 0.05–0.10). Furthermore, excellent short-wave ultraviolet NLO candidate materials also need to possess stable physicochemical properties and excellent crystal growth habits to meet practical application requirements.

[0003] Commercially available ultraviolet NLO crystals, such as BaB₂O₄ (BBO), possess stable physicochemical properties and high-temperature thermal stability, exhibiting excellent transmission range and transmittance, with a second harmonic distortion (HDI) more than five times that of KDP. However, its excessively high birefringence (reaching 0.113 at 1064 nm wavelength) limits the output laser wavelength. LiNbO₃ possesses a more moderate birefringence and is easily grown into large-size, high-quality crystals with stable mechanical and physicochemical properties; however, its narrow transmission range hinders its application in the ultraviolet region. The birefringence of most of these crystals is not within a suitable range, significantly limiting their applications. Therefore, exploring new nonlinear optical crystals with balanced properties is of great significance. Summary of the Invention

[0004] The purpose of this invention is to provide a compound, diglycine trifluoromethanesulfonate, with the chemical formula (C4N2O4H). 11 (CF3SO3), with a molecular weight of 268.144, was prepared by room temperature solution method.

[0005] Another object of the present invention is to provide a nonlinear optical crystal of diglycine trifluoromethanesulfonate, the chemical formula of which is (C4N2O4H). 11 (CF3SO3), molecular weight 268.144, crystal system monoclinic, space group 1. Cc The unit cell parameters are a=14.8353(5) Å, b = 8.9818(3) Å, c = 10.0267(4) Å, α = γ = 90°, β =120.090(1)°, Z = 4, unit cell volume is 1155.99(7) Å 3 .

[0006] Another object of the present invention is to provide diglycine trifluoromethanesulfonate (C4N2O4H 11 Applications of (CF3SO3) nonlinear optical crystals.

[0007] The present invention discloses a compound, diglycine trifluoromethane sulfonate, the chemical formula of which is (C4N2O4H). 11 (CF3SO3), with a molecular weight of 268.144, was prepared by room temperature solution method.

[0008] A nonlinear optical crystal of diglycine trifluoromethane sulfonate, the chemical formula of which is (C4N2O4H). 11 (CF3SO3), belongs to the monoclinic crystal system, space group . Cc The unit cell parameters are a =14.8353(5) Å, b = 8.9818(3) Å, c =10.0267(4) Å, α = γ = 90°, β =120.090(1)°, Z = 4, unit cell volume is 1155.99(7) Å 3 .

[0009] The preparation method of the diglycine trifluoromethane sulfonate nonlinear optical crystal involves using a room temperature solution method, a solvothermal method, and a water bath heating method to prepare the nonlinear optical crystal. The specific operation is carried out according to the following steps: Crystal preparation by room temperature solution method: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Filter the mixed solution from step a using qualitative filter paper, then seal it with a PVC 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. Then let it stand at room temperature for 5–15 days to obtain millimeter-sized C4N2O4H. 11 (CF3SO3) Nonlinear optical crystal; Solvothermal preparation of crystals: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Transfer the solution from 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 60-80 ℃ at a rate of 5-20℃ / h, keep the temperature constant for 5 days, and then lower the temperature to room temperature at a rate of 5-10℃ / day. d. Open the high-pressure reactor to obtain millimeter-sized C4N2O4H. 11 (CF3SO3) Nonlinear optical crystal; Crystal preparation by water bath heating method: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Seal the container containing the solution from step a with weighing paper and place it in a static environment free from shaking, contamination, and air convection. Prick several small holes in the seal to adjust the evaporation rate of the water in the aqueous solution. Let it stand at room temperature for 5-10 days to obtain the product (C4N2O4H). 11 Polycrystalline powder of (CF3SO3); c. The (C4N2O4H) obtained in step b 11 (CF3SO3) polycrystalline powder was placed in a polytetrafluoroethylene beaker, deionized water was added, and the mixture was stirred until it was fully dissolved to obtain a mixed solution. d. Seal the mixed solution obtained in step c with a polyvinyl chloride film, making several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Then place the beaker in a water bath at a temperature of 60–80℃. After the growth is complete, centimeter-sized (C4N2O4H) crystals are obtained. 11 (CF3SO3) Nonlinear optical crystal.

[0010] The diglycine trifluoromethane sulfonate nonlinear optical crystal is used in the fabrication of nonlinear optical devices, frequency multipliers, up or down frequency converters, or optical parametric oscillators.

[0011] This invention relates to a compound, diglycine trifluoromethanesulfonate, and a diglycine trifluoromethanesulfonate nonlinear optical crystal, along with their preparation method and applications. The diglycine trifluoromethanesulfonate (C4N2O4H) in this crystal... 11 The ultraviolet cutoff edge of (CF3SO3) is 216 nm.

[0012] At a wavelength of 546 nm, diglycine trifluoromethanesulfonate (C4N2O4H) 11 The theoretically calculated birefringence of (CF3SO3) is 0.078.

[0013] At a fundamental laser wavelength of 1064 nm, diglycine trifluoromethanesulfonate (C4N2O4H) 11 (CF3SO3) exhibits strong second harmonic efficiency and type I matching behavior comparable to KDP.

[0014] The preparation method of the diglycine trifluoromethane sulfonate nonlinear optical crystal described in this invention is simple and easy to operate, and exhibits excellent optical performance, ideal birefringence, wide transmission range and moderate second harmonic effect, and can be regarded as a class of high-performance ultraviolet nonlinear optical crystals.

[0015] The diglycine trifluoromethane sulfonate nonlinear optical crystal of this invention is prepared using conical flasks, beakers, or hydrothermal reactors lined with polytetrafluoroethylene. When using conical flasks or beakers, the containers must first be cleaned with acid, then rinsed with deionized water, and finally dried.

[0016] The present invention relates to a compound, diglycine trifluoromethane sulfonate, and a diglycine trifluoromethane sulfonate nonlinear optical crystal, as well as their preparation method and uses. The diglycine trifluoromethane sulfonate contains a glycine C2H5NO2 organic π-conjugated unit, and this optically active group has the following advantages: (1) Organic π-conjugated units have a large dipole moment, which helps to enhance the birefringence of crystals; (2) π conjugate units tend to produce significant optical anisotropy differences between the in-plane direction and the direction perpendicular to the plane; (3) By expanding the conjugate frame, polarization anisotropy can be amplified, thereby increasing the birefringence; (4) The organic ligands are rich in hydrogen bonding sites, and the directionality of hydrogen bonds promotes the assembly of birefringent active units into a hydrogen-bonded supramolecular framework. Calculations show that the [C2H5NO2] group has a large polarizability anisotropy (δ) and hyperpolarizability (|βmax|).

[0017] The diglycine trifluoromethane sulfonate used in this invention is a novel nonlinear optical crystal that exhibits excellent optical properties, including ideal birefringence, a wide transmission range, and a moderate second harmonic effect. It can serve as a high-performance ultraviolet nonlinear optical crystal.

[0018] The preparation process of this invention features simple reaction conditions, easy operation, easy crystal growth, high product purity, and stable properties. The preparation of the diglycine trifluoromethane sulfonate compound in this invention only requires simple water bath heating, resulting in low energy consumption and making it economical and environmentally friendly. Attached Figure Description

[0019] Figure 1 The compound of this invention (C4N2O4H) 11 The performance characterization diagrams of (CF3SO3) are shown, where a represents (C4N2O4H) 11 Powder XRD pattern of (CF3SO3); b is (C4N2O4H 11 c) is the second harmonic intensity diagram of (CF3SO3) compared with KDP at 1064nm; d is the theoretically calculated birefringence diagram; d is the ultraviolet cutoff edge diagram after ultraviolet / visible / infrared diffuse reflectance test. Figure 2 This invention (C4N2O4H) 11 Schematic diagram of a large-size crystal of (CF3SO3); Figure 3 This invention (C4N2O4H) 11 This diagram illustrates the working principle of a nonlinear optical device fabricated from (CF3SO3) crystal, where 1 represents the laser, 2 represents the emitted beam, and 3 represents (C4N2O4H) crystal. 11 (CF3SO3) crystal, 4 is the emitted beam, and 5 is the filter.

[0020] The present invention will be further described below with reference to the embodiments. It should be noted that the following embodiments should not be construed as limiting the scope of protection of the present invention, and any improvements made on the basis of the present invention will not violate the spirit of the present invention.

[0021] Unless otherwise specified, all raw materials and equipment used in this invention are commercially available. Example 1

[0022] Preparation of compounds: According to the reaction equation: 2C2H5NO2 + CF3SO3H → (C4N2O4H 11 (CF3SO3) was used to synthesize diglycine trifluoromethanesulfonate (C4N2O4H) via a room temperature solution method. 11 (CF3SO3): a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Filter the mixed solution from step a with qualitative filter paper, then seal it 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. Then let it stand at room temperature for 7 days to obtain the compound diglycine trifluoromethane sulfonate. Example 2

[0023] Synthetic preparation of (C4N2O4H) by room temperature solution method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Filter the mixed solution from step a using qualitative filter paper, then seal it with a polyvinyl chloride film. 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. Then let it stand at room temperature for 5 days to obtain (C4N2O4H) with dimensions of 4mm × 2mm × 1mm. 11 (CF3SO3) Nonlinear optical crystal. Example 3

[0024] Synthetic preparation of (C4N2O4H) by room temperature solution method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Filter the mixed solution from step a using qualitative filter paper, then seal it with a polyvinyl chloride film. 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. Then let it stand at room temperature for 10 days to obtain (C4N2O4H) with dimensions of 6mm × 3mm × 2mm.11 (CF3SO3) Nonlinear optical crystal. Example 4

[0025] Synthetic preparation of (C4N2O4H) by room temperature solution method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Filter the mixed solution from step a using qualitative filter paper, then seal it with a polyvinyl chloride film. 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. Then let it stand at room temperature for 15 days to obtain (C4N2O4H) with dimensions of 7mm × 4mm × 2mm. 11 (CF3SO3) Nonlinear optical crystal. Example 5

[0026] Solvothermal synthesis of (C4N2O4H) 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Transfer the solution 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 60°C at a rate of 5°C / h, keep it at the temperature for 5 days, and then lower it to room temperature at a rate of 5°C / day. d. Open the high-pressure reactor to obtain (C4N2O4H) with dimensions of 5mm × 3mm × 1mm. 11 (CF3SO3) Nonlinear optical crystal. Example 6

[0027] Solvothermal synthesis of (C4N2O4H) 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Transfer the solution from 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 65°C at a rate of 10°C / h, keep it at the constant temperature for 5 days, and then lower it to room temperature at a rate of 8°C / day. d. Open the high-pressure reactor to obtain (C4N2O4H) with dimensions of 3mm × 2mm × 1mm. 11 (CF3SO3) Nonlinear optical crystal. Example 7

[0028] Solvothermal synthesis of (C4N2O4H) 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Transfer the solution from 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 70°C at a rate of 15°C / h, keep it at the temperature for 5 days, and then lower it to room temperature at a rate of 5°C / day. d. Open the high-pressure reactor to obtain (C4N2O4H) with dimensions of 2mm × 3mm × 1mm. 11 (CF3SO3) Nonlinear optical crystal. Example 8

[0029] Solvothermal synthesis of (C4N2O4H) 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Transfer the solution from 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 80℃ at a rate of 20℃ / h, keep it at the temperature for 5 days, and then lower it to room temperature at a rate of 10℃ / day. d. Open the high-pressure reactor to obtain (C4N2O4H) with dimensions of 4mm × 3mm × 1mm. 11 (CF3SO3) Nonlinear optical crystal. Example 9

[0030] Synthesis of (C4N2O4H) by water bath heating method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Seal the container containing the solution from step a with weighing paper and place it in a static environment free from shaking, contamination, and air convection. Poke several small holes in the seal to adjust the evaporation rate of the water in the aqueous solution. Let it stand at room temperature for 7 days. The resulting product is (C4N2O4H). 11 Polycrystalline powder of (CF3SO3); c. The (C4N2O4H) obtained in step b 11 (CF3SO3) polycrystalline powder was placed in a polytetrafluoroethylene beaker, deionized water was added, and the mixture was stirred until it was fully dissolved to obtain a mixed solution. d. Seal the mixture obtained in step c with a polyvinyl chloride film, and punch several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Then place the beaker in a water bath at 60°C. After the growth is completed, a diglycine trifluoromethane sulfonate nonlinear optical crystal with a size of 12 mm × 4 mm × 1 mm is obtained. Example 10

[0031] Synthesis of (C4N2O4H) by water bath heating method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Seal the container containing the solution from step a with weighing paper and place it in a static environment free from shaking, contamination, and air convection. Poke several small holes in the seal to adjust the evaporation rate of the water in the aqueous solution. Let it stand at room temperature for 7 days. The resulting product is (C4N2O4H). 11 Polycrystalline powder of (CF3SO3); c. The (C4N2O4H) obtained in step b 11 (CF3SO3) polycrystalline powder was placed in a polytetrafluoroethylene beaker, deionized water was added, and the mixture was stirred until it was fully dissolved to obtain a mixed solution. d. Seal the solution obtained in step c with a polyvinyl chloride film, and punch several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Then place the beaker in a water bath at 70°C. After the growth is completed, a diglycine trifluoromethane sulfonate nonlinear optical crystal with a size of 10 mm × 4 mm × 1 mm is obtained. Example 11

[0032] Synthesis of (C4N2O4H) by water bath heating method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Seal the container containing the solution from step a with weighing paper and place it in a static environment free from shaking, contamination, and air convection. Poke several small holes in the seal to adjust the evaporation rate of the water in the aqueous solution. Let it stand at room temperature for 7 days. The resulting product is (C4N2O4H). 11 Polycrystalline powder of (CF3SO3); c. The (C4N2O4H) obtained in step b 11 (CF3SO3) polycrystalline powder was placed in a polytetrafluoroethylene beaker, deionized water was added, and the mixture was stirred until it was fully dissolved to obtain a mixed solution. d. Seal the solution obtained in step c with a polyvinyl chloride film, and punch several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Then place the beaker in a water bath at 75°C. After the growth is completed, a diglycine trifluoromethane sulfonate nonlinear optical crystal with a size of 9 mm × 3 mm × 1 mm is obtained. Example 12

[0033] Synthesis of (C4N2O4H) by water bath heating method 11 (CF3SO3) Nonlinear optical crystal: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Seal the container containing the solution from step a with weighing paper and place it in a static environment free from shaking, contamination, and air convection. Poke several small holes in the seal to adjust the evaporation rate of the water in the aqueous solution. Let it stand at room temperature for 7 days. The resulting product is (C4N2O4H). 11 Polycrystalline powder of (CF3SO3); c. The (C4N2O4H) obtained in step b11 (CF3SO3) polycrystalline powder was placed in a polytetrafluoroethylene beaker, deionized water was added, and the mixture was stirred until it was fully dissolved to obtain a mixed solution. d. Seal the solution obtained in step c with a polyvinyl chloride film, and punch several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Then place the beaker in a water bath at 80°C. After the growth is completed, a diglycine trifluoromethane sulfonate nonlinear optical crystal with a size of 8 mm × 2 mm × 1 mm is obtained. Example 13

[0034] The arbitrary (C4N2O4H) obtained in Examples 2-12 11 (CF3SO3) nonlinear optical crystals are processed according to matching directions, and according to the attached... Figure 3 As shown, the laser is positioned at location 3. At room temperature, a Q-switched Nd:YAG laser is used as the light source, with an incident wavelength of 1064 nm. An infrared beam 2 with a wavelength of 1064 nm emitted from the Q-switched Nd:YAG laser 1 is incident on the (C4N2O4H) laser. 11 (CF3SO3) single crystal 3 produces green frequency-doubled light with a wavelength of 532nm, and the output intensity is about 1 times that of KDP under the same conditions.

Claims

1. A compound, diglycine trifluoromethane sulfonate, characterized in that... The chemical formula of this compound is (C4N2O4H 11 (CF3SO3), with a molecular weight of 268.144, was prepared by room temperature solution method.

2. A diglycine trifluoromethane sulfonate nonlinear optical crystal, characterized in that... The chemical formula of this crystal is (C4N2O4H). 11 (CF3SO3), belongs to the monoclinic crystal system, space group . Cc The unit cell parameters are a =14.8353(5) Å, b = 8.9818(3) Å, c = 10.0267(4) Å, α = γ = 90°, β =120.090(1)°, Z = 4, unit cell volume is 1155.99(7) Å 3 .

3. The method for preparing the diglycine trifluoromethane sulfonate nonlinear optical crystal according to claim 2, characterized in that, Nonlinear optical crystals were prepared using room temperature solution method, solvothermal method, and water bath heating method. The specific operations were carried out according to the following steps: Crystal preparation by room temperature solution method: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Filter the mixed solution from step a with qualitative filter paper, then seal it 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. Then let it stand at room temperature for 5–15 days to obtain the diglycine trifluoromethane sulfonate nonlinear optical crystal. Solvothermal preparation of crystals: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Transfer the solution from 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 60-80 ℃ at a rate of 5-20℃ / h, keep the temperature constant for 5 days, and then lower the temperature to room temperature at a rate of 5-10℃ / day. d. Open the high-pressure reactor to obtain high-quality, large-size transparent (C4N2O4H) particles at the centimeter scale. 11 (CF3SO3) Nonlinear optical crystal; Crystal preparation by water bath heating method: a. Weigh the raw materials (C2H5NO2) and (CF3SO3H) for the synthesis of diglycine trifluoromethane sulfonate at a molar ratio of 2:1 and put them into polytetrafluoroethylene beakers. Mix them evenly, add deionized water, and stir to mix evenly to obtain a mixture. b. Seal the container containing the solution from step a with weighing paper and place it in a static environment free from shaking, contamination, and air convection. Prick several small holes in the seal to adjust the evaporation rate of the water in the aqueous solution. Let it stand at room temperature for 5-10 days to obtain the product (C4N2O4H). 11 Polycrystalline powder of (CF3SO3); c. The (C4N2O4H) obtained in step b 11 (CF3SO3) polycrystalline powder was placed in a polytetrafluoroethylene beaker, deionized water was added, and the mixture was stirred until it was fully dissolved to obtain a mixed solution. d. Seal the mixed solution obtained in step c with a polyvinyl chloride film, and punch several small holes in the seal to adjust the evaporation rate of the solvent in the solution. Then place the beaker in a water bath at a temperature of 60-80℃. After the growth is completed, a large-sized diglycine trifluoromethanesulfonate nonlinear optical crystal is obtained.

4. The nonlinear optical crystal of diglycine trifluoromethane sulfonate according to claim 2 is used in the preparation of nonlinear optical devices, frequency multipliers, up or down frequency converters, or optical parametric oscillators.

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