CN114074928A - Strontium sulfamate, strontium sulfamate nonlinear optical crystal, and preparation method and application thereof - Google Patents

Strontium sulfamate, strontium sulfamate nonlinear optical crystal, and preparation method and application thereof Download PDF

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CN114074928A
CN114074928A CN202010803194.4A CN202010803194A CN114074928A CN 114074928 A CN114074928 A CN 114074928A CN 202010803194 A CN202010803194 A CN 202010803194A CN 114074928 A CN114074928 A CN 114074928A
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strontium
strontium sulfamate
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CN114074928B (en
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叶宁
罗敏
郝霞
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Fujian Institute of Research on the Structure of Matter of CAS
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    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
    • C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
    • C01B21/096—Amidosulfonic acid; Salts thereof
    • C—CHEMISTRY; METALLURGY
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    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract

The invention discloses a strontium sulfamate compound, a strontium sulfamate nonlinear optical crystal, and a preparation method and application thereof. Sr (NH)2SO3)2The structure of the crystal belongs to monoclinic system, the space group is Pc, and the unit cell parameter is
Figure DDA0002628149870000011
α ═ γ ═ 90 °, β ═ 107.803(9), Z ═ 2; unit cell volume of
Figure DDA0002628149870000012
Meanwhile, the frequency doubling effect of the powder is 1.2 times of KDP, and the ultraviolet absorption edge of the powder is shorter than that of KDP200nm, and can be used for a 2-6 frequency harmonic generator of Nd: YAG (lambda is 1.064 μm). The strontium sulfamate single crystal is colorless and transparent, does not deliquesce and has good chemical stability, and can be widely applied to various nonlinear optical fields.

Description

Strontium sulfamate, strontium sulfamate nonlinear optical crystal, and preparation method and application thereof
Technical Field
The invention belongs to the field of photoelectron functional materials, relates to a novel photoelectron functional material, a preparation method and application thereof, and particularly relates to strontium sulfamate, a strontium sulfamate nonlinear optical crystal, a preparation method and application thereof.
Background
Nonlinear optical crystals have been developed over decades and the frequency conversion range now has been able to cover substantially the entire optical band from deep ultraviolet to mid-infrared. However, from the practical point of view, no practical frequency doubling crystal exists in the deep ultraviolet region below 200 nm. For generating deep ultraviolet laser, near infrared fundamental wave laser sources such as Nd: YAG, Nd: YVO are commonly used4And the like, and generates higher harmonics by frequency conversion of the nonlinear optical crystal. However, the wavelength difference from near infrared to deep ultraviolet is large, and in order to reduce the frequency conversion times and improve the total conversion efficiency, a direct frequency doubling method must be adopted as much as possible. However, the nonlinear optical crystal capable of realizing direct frequency doubling in deep ultraviolet region below 200nm is KBe2BO3F2(KBBF) and Sr2Be2B2O7(SBBO), but both of these crystals have not been promoted and used at present because of the difficulty in growth.
Due to the lack of practical deep ultraviolet frequency doubling crystals, the deep ultraviolet region below 200nm is the last wavelength range which cannot be covered by the commercial all-solid-state laser at present, however, the band frequency doubling crystals have important application requirements in the aspects of semiconductor lithography technology, laser spectroscopy, biophysics, photoelectron spectroscopy, laser medicine and the like. At present, an excimer laser is generally adopted as a light source, but due to the defects of the excimer laser, the excimer laser is replaced by an all-solid-state laser which is small in size, reliable, durable and good in light beam quality. In recent years, the demand for all-solid-state deep ultraviolet lasers with small power has been strong. Therefore, the development of the practical deep ultraviolet frequency doubling crystal can not only fill the blank of the nonlinear optical frequency doubling material in the deep ultraviolet region, but also effectively promote the development of related subjects and industrial technologies.
Disclosure of Invention
In order to improve the technical problem, the invention provides a strontium sulfamate compound, the chemical formula of which is Sr (NH)2SO3)2。
The invention also provides a preparation method of the strontium sulfamate compound, which comprises the step of mixing SrCO3And NH2SO3H, reacting to obtain the strontium sulfamate compound.
According to an embodiment of the invention, the SrCO3And NH2SO3The molar ratio of H can be 1 (2-2.5), preferably 1 (2.1-2.4); exemplary are 1:2, 1:2.2, 1: 2.5.
According to an embodiment of the invention, the reaction is carried out in a solvent, which may be selected from organic or inorganic solvents, preferably inorganic solvents, such as water, exemplified by deionized water.
According to an embodiment of the invention, the total mass of the starting material (i.e. SrCO)3And NH2SO3The sum of the masses of H) and the solvent in a volume ratio of (50-80) g to 100mL, preferably (50-60) g to 100 mL; exemplary are 50g:100mL, 57g:100mL, 60g:100mL, 70g:100mL, 80g:100 mL.
According to an embodiment of the present invention, the temperature of the reaction may be 40 to 100 ℃, preferably 50 to 90 ℃, exemplary 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃.
According to an embodiment of the present invention, the reaction time may be 1 to 10 days, preferably 3 to 7 days, and exemplary are 3 days, 4 days, 5 days, 6 days, and 7 days.
According to an embodiment of the invention, the preparation method further comprises: and collecting the strontium sulfamate compound from the reaction solution after the reaction is finished.
The invention also provides a nonlinear optical crystal which is strontium sulfamate Sr (NH)2SO3)2And (4) crystals.
According to an embodiment of the invention, said Sr (NH)2SO3)2The crystal has an X-ray powder diffraction pattern substantially as shown in figure 3.
According to an embodiment of the invention, said Sr (NH)2SO3)2The crystal has no symmetry center, belongs to monoclinic system, and has Pc space groupCell parameter of
Figure BDA0002628149850000021
Figure BDA0002628149850000031
α＝γ＝90°，β＝107.803(9)。
According to an embodiment of the invention, said Sr (NH)2SO3)2The number of molecules in the crystal unit cell, Z, is 2.
According to an embodiment of the invention, said Sr (NH)2SO3)2Unit cell volume of the crystal is
Figure BDA0002628149850000032
Figure BDA0002628149850000033
According to an embodiment of the invention, said Sr (NH)2SO3)2The powder frequency doubling effect of the crystal is KH2PO4(KDP) 1.2 times higher.
According to an embodiment of the invention, said Sr (NH)2SO3)2The ultraviolet absorption edge of the crystal is shorter than 200 nm. I.e. Sr (NH)2SO3)2The crystal is a deep ultraviolet frequency doubling optical crystal.
According to an embodiment of the invention, said Sr (NH)2SO3)2The crystals were colorless transparent crystals. Further, the volume of the crystal may be greater than 2.0mm3E.g. greater than 3mm3。
According to an embodiment of the invention, said Sr (NH)2SO3)2The crystal has a crystal structure as shown in fig. 2.
The present invention also provides the above Sr (NH)2SO3)2A preparation method of the crystal, which comprises the preparation method of the strontium sulfamate compound.
Preferably, the reaction solution obtained after completion of the reaction may be evaporated at a constant temperature to obtain Sr (NH)2SO3)2And (4) crystals. For example, the temperature of the evaporation is 50 to 70 ℃, preferably 55 to 65 ℃, and exemplary 60 ℃. For example, the evaporation time may be 2 to 10 days, such as 2.5 to 8 days, with 7 days being exemplary.
According to an embodiment of the invention, said Sr (NH)2SO3)2The volume of the crystal may be greater than 2.0mm3E.g. greater than 3mm3。
The invention also provides the application of the strontium sulfamate compound and/or the strontium sulfamate crystal in an optical device. For example, it can be used for frequency conversion of laser output of a laser, a harmonic generator in an ultraviolet region, an optical parametric and amplification device, or an optical waveguide device. Preferably, the strontium sulfamate compound and/or the strontium sulfamate crystal can be used for generating 2-frequency, 3-frequency, 4-frequency, 5-frequency or 6-frequency harmonic light output for a laser beam with the wavelength of 1.064 μm.
Preferably, the strontium sulfamate compound and/or the strontium sulfamate crystal can be used for optical parametric and amplification devices from the infrared to ultraviolet regions.
The invention also provides an optical device which contains the strontium sulfamate compound and/or the strontium sulfamate crystal.
According to embodiments of the present invention, the optical device may be a laser, a harmonic generator, an optical parametric and amplification device, or an optical waveguide device; preferably a laser; more preferably, the laser is an all-solid-state laser.
Illustratively, an all-solid-state laser contains the strontium sulfamate compound and/or the Sr (NH)2SO3)2And (4) crystals. Preferably, the all-solid-state laser is an all-solid-state deep ultraviolet laser.
The invention has the beneficial effects that:
(1) the invention provides a chemical formula of Sr (NH)2SO3)2The strontium sulfamate compound, the strontium sulfamate nonlinear optical crystal, the preparation method and the application thereof, and the Sr (NH) is measured by adopting a powder frequency doubling test method2SO3)2The phase matching ability of the powder is KH2PO41.2 times of (KDP), thus indicating that Sr (NH) is produced according to the present invention2SO3)2The strontium sulfamate nonlinear optical crystal has better phase matching capability; and its ultraviolet absorption edge is shorter than 200nm, so that Sr (NH)2SO3)2The nonlinear optical crystal can realize 2 frequency multiplication of Nd, YAG (lambda is 1.064 mu m); and, Sr (NH) can be predicted2SO3)2The crystal can be used for harmonic generators of 3, 4, 5 and 6 frequency doubling of Nd: YAG, and even for generating harmonic light output shorter than 200 nm.
(2) Sr (NH) prepared by the invention2SO3)2The single crystal is colorless and transparent, does not deliquesce and has good chemical stability, so the single crystal is expected to be widely applied in various nonlinear optical fields, and the application of nonlinear optical crystal materials in deep ultraviolet bands is developed to promote the development of related subjects and industrial technologies.
Drawings
FIG. 1 shows Sr (NH) obtained in example 12SO3)2X-ray powder diffraction pattern of single crystal.
FIG. 2 shows Sr (NH)2SO3)2Schematic diagram of unit cell structure of crystal.
FIG. 3 shows Sr (NH)2SO3)2The crystal is used as a typical schematic diagram of nonlinear optical effect when being applied as a frequency doubling crystal, wherein 1 is a laser, 2 is an incident laser beam, 3 is a single crystal of example 2 subjected to crystal post-treatment and optical processing, 4 is an emergent laser beam, and 5 is a filter.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
The Sr (NH) obtained in the following examples was paired with a Cu target equipped with a physical Mini-flex 600 powder diffractometer2SO3)2Carrying out characterization on the single crystal; and (3) testing conditions are as follows: and (4) room temperature.
Example 1
Preparation of Sr (NH) by constant temperature evaporation reaction2SO3)2(Single Crystal)
Preparation of Sr (NH)2SO3)2Raw materials for single crystal: SrCO3 0.74g(0.005mol)
NH2SO3H 0.97g(0.011mol)
The specific operation steps are as follows: weighing the raw materials in the operation box according to the dosage, uniformly mixing, adding into a 25mL beaker, adding 3mL deionized water, placing the beaker into an oven, slowly heating the oven to 60 ℃, and evaporating at constant temperature for 3 days to obtain Sr (NH) (2.5 × 1 × 0.8 mm)2SO3)2And (3) single crystal.
Sr (NH) produced in this example2SO3)2The X-ray powder diffraction pattern of the single crystal is shown in figure 1, and the results in the figure show that: sr (NH) obtained in this example2SO3)2The single crystal is a single pure phase and has high purity.
The schematic diagram of its unit cell structure is shown in FIG. 2. Obtained Sr (NH)2SO3)2The single crystal has no symmetry center, belongs to monoclinic system, has space group of Pc and unit cell parameter of
Figure BDA0002628149850000051
Figure BDA0002628149850000052
α ═ γ ═ 90 °, β ═ 107.803(9), Z ═ 2; unit cell volume of
Figure BDA0002628149850000053
Example 2
Preparation of Sr (NH) by constant temperature evaporation reaction2SO3)2(Single Crystal)
Preparation of Sr (NH)2SO3)2Raw materials for single crystal: SrCO3 36.91g(0.25mol)
NH2SO3H 53.40g(0.55mol)
The specific operation steps are as follows: weighing the raw materials in the operation box according to the dosage, uniformly mixing, then placing into a 300mL beaker, adding 150mL deionized water, placing the beaker into an oven, slowly heating the oven to 60 ℃, and evaporating at constant temperature for 7 days to obtain Sr (NH) with the size of 3 x 1.2 x 1mm2SO3)2And (3) single crystal.
Example 3
For Sr (NH) obtained in example 22SO3)2The crystal samples were subjected to frequency doubling test experiments as shown in fig. 3.
Sr (NH) obtained in example 22SO3)2The crystal is cut, oriented, polished and placed in position 3 in the apparatus shown in FIG. 3. YAG laser is used as an input light source (namely a laser 1) at room temperature, the incident wavelength of an incident laser beam 2 is 1064nm, and after the incident laser beam 2 is subjected to crystal post-treatment and optical processing, the single crystal 3 in the embodiment 2 is observed, and an emergent laser beam 4 is obviously output as 532nm frequency-doubled green light after passing through a filter 5. Sr (NH)2SO3)2The output intensity (powder frequency doubling effect) of the method is about 1.2 times of KDP under the same condition.
Example 4
Different from the embodiment 3, the frequency doubling light of the Q-switched Nd: YAG laser is used as an input light source, the incident wavelength is 532nm, and obvious 266nm frequency doubling ultraviolet light output is observed.
Example 5
Different from the embodiment 3, the frequency tripling double-frequency light of the Q-switched Nd-YAG laser is used as an input light source, the incident wavelength is 355nm, and 177.3nm frequency doubled deep ultraviolet light output can be observed.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A strontium sulfamate compound is characterized in that the chemical formula of the strontium sulfamate compound is Sr (NH)2SO3)2。
2. A process for preparing strontium sulfamate compounds according to claim 1, which comprises reacting SrCO3And NH2SO3H, reacting to obtain the strontium sulfamate compound.
3. The method of claim 2, wherein the SrCO3And NH2SO3The molar ratio of H is 1 (2-2.5), preferably 1 (2.1-2.4);
preferably, the reaction is carried out in a solvent selected from an organic or inorganic solvent, preferably an inorganic solvent, such as water;
preferably, the total mass of the starting materials (i.e., SrCO)3And NH2SO3The sum of the masses of H) and the solvent in a volume ratio of (50-80) g to 100mL, preferably (50-60) g to 100 mL;
preferably, the reaction temperature is 40-100 ℃, preferably 50-90 ℃;
preferably, the reaction time is 1-10 days, preferably 3-7 days;
preferably, the preparation method further comprises: and collecting the strontium sulfamate compound from the reaction solution after the reaction is finished.
4. The nonlinear optical crystal is characterized in that strontium sulfamate Sr (NH)2SO3)2And (4) crystals.
5. The nonlinear optical crystal according to claim 4, wherein the Sr (NH)2SO3)2The crystal has a shape substantially as shown in FIG. 3An X-ray powder diffraction pattern as shown;
preferably, the Sr (NH)2SO3)2The crystal has no symmetry center, belongs to monoclinic system, has space group of Pc and unit cell parameter of
Figure FDA0002628149840000011
α＝γ＝90°，β＝107.803(9)；
Preferably, the Sr (NH)2SO3)2The number of molecules Z in the crystal unit cell is 2;
preferably, the Sr (NH)2SO3)2Unit cell volume of the crystal is
Figure FDA0002628149840000012
Preferably, the Sr (NH)2SO3)2The powder frequency doubling effect of the crystal is KH2PO41.2 times (KDP);
preferably, the Sr (NH)2SO3)2The ultraviolet absorption edge of the crystal is shorter than 200 nm;
preferably, the Sr (NH)2SO3)2The crystal is colorless transparent crystal; further, the volume of the crystal is more than 2.0mm3；
Preferably, the Sr (NH)2SO3)2The crystal has a crystal structure as shown in fig. 2.
6. The Sr (NH) of any one of claims 4 to 52SO3)2A method for producing a crystal, comprising the step of producing a strontium sulfamate compound according to claim 2 or 3.
7. The production method according to claim 6, wherein the reaction solution obtained after completion of the reaction is evaporated at a constant temperature to obtain Sr (NH)2SO3)2A crystal;
preferably, the temperature of the evaporation is 50-70 ℃, preferably 55-65 ℃;
preferably, the evaporation time is 2-10 days, such as 2.5-8 days.
Preferably, the Sr (NH)2SO3)2The volume of the crystal is more than 2.0mm3。
8. Use of a strontium sulfamate compound according to claim 1 and/or a strontium sulfamate compound obtained by the production method according to any one of claims 2 to 3 and/or a strontium sulfamate crystal according to any one of claims 4 to 5 and/or a strontium sulfamate crystal obtained by the production method according to any one of claims 6 to 7 in an optical device;
for example, it is used for frequency conversion of laser output of a laser, a harmonic generator of an ultraviolet region, an optical parametric and amplification device, or an optical waveguide device;
preferably, it is used for generating a 2-, 3-, 4-, 5-or 6-frequency doubled harmonic light output for a laser beam having a wavelength of 1.064 μm.
Preferably, it is used for optical parametric and amplification devices from the infrared to ultraviolet region.
9. An optical device comprising the strontium sulfamate compound according to claim 1, the strontium sulfamate compound produced by the method according to any one of claims 2 to 3, and/or the Sr (NH) produced by the production method according to any one of claims 4 or 5 and claims 6 to 72SO3)2A crystal;
preferably, the optical device is a laser, a harmonic generator, an optical parametric and amplification device or an optical waveguide device; preferably a laser; more preferably, the laser is an all-solid-state laser.
10. An all-solid-state laser comprising the strontium sulfamate compound according to claim 1, the strontium sulfamate compound produced by the method according to any one of claims 2 to 3, and/or the Sr (NH) according to claim 4 or 52SO3)2Crystals of the Sr (NH) obtained by the production method according to any one of claims 6 to 72SO3)2A crystal;
preferably, the all-solid-state laser is an all-solid-state deep ultraviolet laser.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4260593A (en) * 1979-03-08 1981-04-07 Hoechst Aktiengesellschaft Process for the manufacture of ammonium sulfamate
CN1590283A (en) * 2003-08-28 2005-03-09 尚士清 Preparation of metal aminosulfonate
CN1592867A (en) * 2001-05-17 2005-03-09 大金工业株式会社 Nonlinear optical material comprising fluorine-containing polymer
CN109803952A (en) * 2016-10-19 2019-05-24 魁北克电力公司 Sulfamic acid derivatives and preparation method thereof
CN110042465A (en) * 2018-01-17 2019-07-23 中国科学院福建物质结构研究所 Alkaline-earth metal borofluoride compound, crystal, preparation method and purposes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4260593A (en) * 1979-03-08 1981-04-07 Hoechst Aktiengesellschaft Process for the manufacture of ammonium sulfamate
CN1592867A (en) * 2001-05-17 2005-03-09 大金工业株式会社 Nonlinear optical material comprising fluorine-containing polymer
CN1590283A (en) * 2003-08-28 2005-03-09 尚士清 Preparation of metal aminosulfonate
CN109803952A (en) * 2016-10-19 2019-05-24 魁北克电力公司 Sulfamic acid derivatives and preparation method thereof
CN110042465A (en) * 2018-01-17 2019-07-23 中国科学院福建物质结构研究所 Alkaline-earth metal borofluoride compound, crystal, preparation method and purposes

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
M.H.KUOK: "Vibrational modes of strontium sulphamate crystals", JURNAL FIZIK MALAYSIA, vol. 7, pages 152 - 157 *

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