CN-122010794-A - Compound diglycine trifluoro methane sulfonate and diglycine trifluoro methane sulfonate nonlinear optical crystal, preparation method and application

Abstract

The invention relates to a compound of diglycine trifluoro methane sulfonate and diglycine trifluoro methane sulfonate nonlinear optical crystal, a preparation method and application thereof. The compound is characterized in that the compound is characterized by a chemical formula (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ) of diglycine trifluoromethane sulfonate, a molecular weight of 268.144, a chemical formula of crystal is (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ), a monoclinic system is formed, a space group is Cc, unit cell parameters are a= 14.8353 (5) a, b= 8.9818 (3) a, c= 10.0267 (4) a, alpha=gamma=90 DEG, beta= 120.090 (1) °, Z=4, a unit cell volume is 1155.99 (7) a 3 , and the crystal is prepared by a room temperature solution method, a solvothermal method and a water bath heating method, the process flow is simple and easy to operate, and the crystal shows excellent optical performance, including ideal double refractive index, a short ultraviolet absorption edge of about 216 nm and moderate frequency doubling effect of about 1 time of KH 2 PO 4 (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 to be applied to all-solid-state lasers.

Inventors

• PAN SHILIE
• AN SHUAI
• HOU XUELING

Assignees

• 中国科学院新疆理化技术研究所

Dates

Publication Date

20260512

Application Date

20260203

Claims (4)

1. 1. A compound diglycine trifluoromethane sulfonate is characterized in that the chemical formula of the compound is (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ), the molecular weight is 268.144, and the compound is prepared by adopting a room temperature solution method.
2. 2. A non-linear optical crystal of diglycine trifluoromethane sulfonate, characterized in that the chemical formula of the crystal is (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ), belongs to monoclinic system, space group is Cc, unit cell parameters are a= 14.8353 (5) a, b= 8.9818 (3) a, c= 10.0267 (4) a, α=γ=90°, β= 120.090 (1) °, z=4, and unit cell volume is 1155.99 (7) a 3 .
3. 3. The method for preparing the nonlinear optical crystal of the diglycine trifluoromethane sulfonate according to claim 2, wherein the nonlinear optical crystal is prepared by adopting a room temperature solution method, a solvothermal method and a water bath heating method, and the specific operation is carried out according to the following steps: Preparing crystals by a room temperature solution method: a. Weighing synthetic raw materials (C 2 H 5 NO 2 ) and (CF 3 SO 3 H) of the diglycine trifluoromethane sulfonate according to a molar ratio of 2:1, respectively putting into a polytetrafluoroethylene beaker, uniformly mixing, adding deionized water, and uniformly stirring to obtain a mixed solution; b. Filtering the mixed solution in the step a by using qualitative filter paper, sealing by using a polyvinyl chloride film, placing the mixed solution in a static environment without shaking, pollution and air convection, punching a plurality of small holes in the sealing to adjust the volatilization rate of the solvent in the solution, and standing for 5-15 days at room temperature to obtain the non-linear optical crystal of the diglycine trifluoromethane sulfonate; preparing crystals by a solvothermal method: a. Weighing synthetic raw materials (C 2 H 5 NO 2 ) and (CF 3 SO 3 H) of the diglycine trifluoromethane sulfonate according to a molar ratio of 2:1, respectively putting into a polytetrafluoroethylene beaker, uniformly mixing, adding deionized water, and uniformly stirring to obtain a mixed solution; b. transferring the solution in the step a into a clean and pollution-free lining of a high-pressure reaction kettle with the volume of 100 mL, and screwing and sealing the reaction kettle; c. placing the high-pressure reaction kettle in a constant temperature box, heating to 60-80 ℃ at the rate of 5-20 ℃ per hour, keeping the temperature for 5 days, and then cooling to room temperature at the cooling rate of 5-10 ℃ per day; d. Opening the high-pressure reaction kettle to obtain the centimeter-level high-quality large-size transparent (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ) nonlinear optical crystal; Preparing crystals by a water bath heating method: a. Weighing synthetic raw materials (C 2 H 5 NO 2 ) and (CF 3 SO 3 H) of the diglycine trifluoromethane sulfonate according to a molar ratio of 2:1, respectively putting into a polytetrafluoroethylene beaker, uniformly mixing, adding deionized water, and uniformly stirring to obtain a mixed solution; b. C, sealing the container filled with the solution in the step a by using weighing paper, placing the container in a static environment without shaking, pollution and air convection, punching a plurality of small holes in the sealing for adjusting the evaporation rate of water in the aqueous solution, and standing for 5-10 days at room temperature to obtain polycrystalline powder with a product of (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ); c. B, putting the polycrystalline powder (C 4 N 2 O 4 H 11 )(CF 3 SO 3 ) obtained in the step b into a polytetrafluoroethylene beaker, adding deionized water, stirring and uniformly mixing to fully mix and dissolve the polycrystalline powder to obtain a mixed solution; d. C, sealing the mixed solution obtained in the step C by using a polyvinyl chloride film, punching a plurality of small holes in the seal to adjust the volatilization rate of the solvent in the solution, and then placing the beaker in a water bath kettle at the temperature of 60-80 ℃ until the growth is finished, thus obtaining the large-size di-glycine-trifluoro methane sulfonate nonlinear optical crystal.
4. 4. The nonlinear optical crystal of the compound diglycine trifluoromethane sulfonate according to claim 2, wherein a frequency doubling generator, an upper or lower frequency converter or an optical parametric oscillator is prepared in the preparation of nonlinear optical devices.

Description

Compound diglycine trifluoro methane sulfonate and diglycine trifluoro methane sulfonate nonlinear optical crystal, preparation method and application Technical Field The invention relates to a compound of diglycine trifluoro methane sulfonate and diglycine trifluoro methane sulfonate nonlinear optical crystal, a preparation method and application thereof. Background Nonlinear optical (NLO) crystals play a key role in solid state laser frequency conversion. During the last decades, researchers have found a range of NLO crystals, such as β -BaB 2O4 (β-BBO), LiNbO3 and KH 2PO4 (KDP). However, to meet the needs of laser science and technology development, it is still critical to continue to develop new NLO crystals, particularly crystals suitable for the short wavelength Ultraviolet (UV) region. From the structural design point of view, the ideal shortwave ultraviolet NLO candidate material should meet the following requirements that 1) the shortwave ultraviolet NLO candidate material has a non-central symmetrical structure, 2) the ultraviolet absorption cutoff wavelength is short (lambda cutoff < 280 nm), 3) the large second harmonic response (not less than 1 xKDP) and 4) the appropriate birefringence (delta n=0.05-0.10). In addition, the excellent short wave ultraviolet NLO candidate material also needs to have stable physical and chemical properties and excellent crystal growth habit so as to meet the practical application requirements. Commercial ultraviolet NLO crystal BaB 2O4 (BBO) has stable physical and chemical properties and high-temperature stability, and has very excellent transmission range and transmission rate, and the second harmonic effect is more than five times that of KDP. However, its excessively high birefringence (up to 0.113 at 1064 nm wavelength) limits the output lasing wavelength. LiNbO 3 has a moderate birefringence, and can easily grow large-size high-quality crystals, so that the crystal mechanical and physical and chemical properties are stable, but the narrow transmission range of LiNbO 3 makes the LiNbO difficult to realize application in the ultraviolet region. The birefringence of these crystals is mostly not in the proper range, greatly limiting their applications. It is therefore of great importance to explore new nonlinear optical crystals with balanced properties. Disclosure of Invention The invention aims to provide a compound diglycine trifluoromethane sulfonate, which has a chemical formula of (C 4N2O4H11)(CF3SO3) and a molecular weight of 268.144 and is prepared by adopting a room temperature solution method. Another object of the present invention is to provide a non-linear optical crystal of diglycine trifluoromethane sulfonate having a chemical formula of (C 4N2O4H11)(CF3SO3), a molecular weight of 268.144, a monoclinic system, a space group of Cc, a unit cell parameter of a= 14.8353 (5) a, b= 8.9818 (3) a, c= 10.0267 (4) a, α=γ=90°, β= 120.090 (1) °, z=4, and a unit cell volume of 1155.99 (7) a, 3. It is a further object of the present invention to provide the use of a non-linear optical crystal of diglycine trifluoromethane sulfonate (C 4N2O4H11)(CF3SO3). The chemical formula of the compound is (C 4N2O4H11)(CF3SO3), the molecular weight is 268.144, and the compound is prepared by adopting a room temperature solution method. A non-linear optical crystal of diglycine trifluoromethane sulfonate, the chemical formula of the crystal is (C 4N2O4H11)(CF3SO3), belongs to monoclinic system, space group is Cc, unit cell parameters are a= 14.8353 (5) a, b= 8.9818 (3) a, c= 10.0267 (4) a, α=γ=90°, β= 120.090 (1) °, z=4, and unit cell volume is 1155.99 (7) a 3. The preparation method of the non-linear optical crystal of the diglycine trifluoromethane sulfonate adopts a room temperature solution method, a solvothermal method and a water bath heating method to prepare the non-linear optical crystal, and comprises the following specific operations: Preparing crystals by a room temperature solution method: a. Weighing synthetic raw materials (C 2H5NO2) and (CF 3SO3 H) of the diglycine trifluoromethane sulfonate according to a molar ratio of 2:1, respectively putting into a polytetrafluoroethylene beaker, uniformly mixing, adding deionized water, and uniformly stirring to obtain a mixed solution; b. Filtering the mixed solution in the step a by using qualitative filter paper, sealing by using a polyvinyl chloride film, placing the mixed solution in a static environment without shaking, pollution and air convection, punching a plurality of small holes in the sealing to adjust the volatilization rate of the solvent in the solution, and standing for 5-15 days at room temperature to obtain a millimeter-sized C 4N2O4H11)(CF3SO3) nonlinear optical crystal; preparing crystals by a solvothermal method: a. Weighing synthetic raw materials (C 2H5NO2) and (CF 3SO3 H) of the diglycine trifluoromethane sulfonate according to a molar ratio of 2:1, respectively putting into a polytetrafluoroethy