CN114074928B - Strontium sulfamate, strontium sulfamate nonlinear optical crystal, preparation method and application thereof - Google Patents
Strontium sulfamate, strontium sulfamate nonlinear optical crystal, preparation method and application thereof Download PDFInfo
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- CN114074928B CN114074928B CN202010803194.4A CN202010803194A CN114074928B CN 114074928 B CN114074928 B CN 114074928B CN 202010803194 A CN202010803194 A CN 202010803194A CN 114074928 B CN114074928 B CN 114074928B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
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- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
Abstract
The invention discloses a strontium sulfamate compound, a strontium sulfamate nonlinear optical crystal, a preparation method and application thereof. Sr (NH) 2 SO 3 ) 2 The crystal structure belongs to monoclinic system, the space group is Pc, and the unit cell parameters areα=γ=90°, β= 107.803 (9), z=2; the unit cell volume isMeanwhile, the powder frequency doubling effect is 1.2 times of KDP, and the ultraviolet absorption edge is shorter than 200nm, so that the powder frequency doubling effect can be used for 2-6 frequency doubling harmonic generators of Nd-YAG (lambda=1.064 mu m). The strontium sulfamate monocrystal is colorless and transparent, does not deliquesce, has good chemical stability, and can be widely applied to various nonlinear optical fields.
Description
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 in particular relates to strontium sulfamate and strontium sulfamate nonlinear optical crystals, and a preparation method and application thereof.
Background
Nonlinear optical crystals have been developed for decades, and the range of frequency conversion has now been essentially over the entire optical band from deep ultraviolet to mid-infrared. However, from the practical point of view, there is no frequency doubling crystal which is practically usable in the deep ultraviolet region of 200nm or less. Since the deep ultraviolet laser is generated, it is generally a fundamental laser light source in near infrared, such as Nd: YAG, nd: YVO 4 And the like, higher harmonics are generated by frequency conversion of the nonlinear optical crystal. However, the difference between the near infrared and deep ultraviolet wavelengths is large, and in order to reduce the frequency conversion times and improve the total conversion efficiency, a direct frequency multiplication method must be adopted as much as possible. However, the current nonlinear line capable of realizing direct frequency multiplication of deep ultraviolet region below 200nmThe sexual optical crystal is KBE 2 BO 3 F 2 (KBBF) and Sr 2 Be 2 B 2 O 7 (SBBO), but both crystals are not popularized and applied at present due to the difficulty in growth.
Due to the lack of practical deep ultraviolet frequency doubling crystals, the deep ultraviolet light region below 200nm is the last wavelength range which cannot be covered by the current commercial all-solid-state laser, however, the band frequency doubling crystals have important application requirements in the aspects of semiconductor lithography, laser spectroscopy, biophysics, photoelectron spectroscopy, laser medicine and the like. At present, an excimer laser is generally adopted as a light source in the wave band, but due to the defects of the excimer laser, the excimer laser is replaced by an all-solid-state laser with small volume, reliability, durability and good beam quality. In recent years, the need for low power all-solid-state deep ultraviolet lasers has been strong. Therefore, the development of the practical deep ultraviolet frequency doubling crystal can fill the blank of the nonlinear optical frequency doubling material in the deep ultraviolet region and can forcefully promote the development of relevant disciplines and industrial technologies.
Disclosure of Invention
In order to solve the technical problems, the invention provides a strontium sulfamate compound with a chemical formula of Sr (NH) 2 SO 3 ) 2 。
The invention also provides a preparation method of the strontium sulfamate compound, which comprises the steps of 3 And NH 2 SO 3 H, reacting to obtain the strontium sulfamate compound.
According to an embodiment of the invention, the SrCO 3 And NH 2 SO 3 The molar ratio of H may 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 raw materials (i.e. SrCO 3 And NH 2 SO 3 The sum of the masses of H) to the volume ratio of the solventThe total weight of the catalyst is (50-80) g/100 mL, preferably (50-60) g/100 mL; exemplary are 50g:100mL, 57g:100mL, 60g:100mL, 70g:100mL, 80g:100mL.
According to an embodiment of the present invention, the temperature of the reaction may be 40 to 100 ℃, preferably 50 to 90 ℃, and exemplified by 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃.
According to embodiments of the present invention, the reaction time may be 1 to 10 days, preferably 3 to 7 days, and exemplified by 3 days, 4 days, 5 days, 6 days, 7 days.
According to an embodiment of the present invention, the preparation method further comprises: and collecting the strontium sulfamate compound from the reaction solution after the reaction.
The invention also provides a nonlinear optical crystal which is strontium sulfamate Sr (NH) 2 SO 3 ) 2 And (5) a crystal.
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The crystals have an X-ray powder diffraction pattern substantially as shown in figure 3.
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The crystal has no symmetry center, belongs to monoclinic system, has a space group of Pc and has a unit cell parameter of α＝γ＝90°，β＝107.803(9)。
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The number of molecules in the unit cell of the crystal z=2.
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The unit cell volume of the crystal is
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The powder frequency doubling effect of the crystal is KH 2 PO 4 (KDP) 1.2 times.
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The ultraviolet absorption edge of the crystal is shorter than 200nm. Namely Sr (NH) 2 SO 3 ) 2 The crystal is a deep ultraviolet frequency doubling optical crystal.
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The crystal is colorless transparent crystal. Further, the volume of the crystals may be greater than 2.0mm 3 For example greater than 3mm 3 。
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The crystal has a crystal structure as shown in fig. 2.
The invention also provides the Sr (NH) 2 SO 3 ) 2 The preparation method of the crystal comprises the preparation method of the strontium sulfamate compound.
Preferably, the reaction solution obtained after the completion of the reaction may be evaporated at a constant temperature to obtain Sr (NH) 2 SO 3 ) 2 And (5) a crystal. For example, the temperature of the evaporation is 50-70 ℃, preferably 55-65 ℃, and exemplary 60 ℃. For example, the evaporation time is 2-10 days, for example 2.5-8 days, and exemplary 7 days.
According to an embodiment of the invention, the Sr (NH 2 SO 3 ) 2 The volume of the crystals may be greater than 2.0mm 3 For example greater than 3mm 3 。
The invention also provides the use of the above 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 laser, harmonic generator of ultraviolet region, optical parametric and amplifying device or optical waveguide device. Preferably, the strontium sulfamate compound and/or the strontium sulfamate crystal can be used to produce a 2-, 3-, 4-, 5-, or 6-fold harmonic light output to a laser beam having a wavelength of 1.064 μm.
Preferably, the strontium sulfamate compound and/or the strontium sulfamate crystal can be used for optical parametric and amplifying devices from the infrared to the ultraviolet region.
The invention also provides an optical device containing 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 amplifying 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) 2 SO 3 ) 2 And (5) a crystal. 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 catalyst with a chemical formula of Sr (NH) 2 SO 3 ) 2 Strontium sulfamate compound, strontium sulfamate nonlinear optical crystal, preparation method and application thereof, and Sr (NH) is measured by adopting a powder frequency doubling test method 2 SO 3 ) 2 Is characterized by KH as the powder frequency doubling effect 2 PO 4 1.2 times (KDP), thus indicating that Sr (NH) 2 SO 3 ) 2 The strontium sulfamate nonlinear optical crystal has better phase matching capability; at the same time, the ultraviolet absorption edge is shorter than 200nm, thus Sr (NH) 2 SO 3 ) 2 The nonlinear optical crystal can realize 2 times frequency of Nd: YAG (lambda=1.064 μm); and, sr (NH) 2 SO 3 ) 2 The crystal can be used for a harmonic generator of Nd: YAG frequency 3, 4, 5, 6, or even for generating a harmonic light output shorter than 200nm.
(2) Sr (NH) prepared by the invention 2 SO 3 ) 2 The monocrystal is colorless and transparent, does not deliquesce, has good chemical stability, is hopeful to be widely applied in various nonlinear optical fields,and the application of the nonlinear optical crystal material in the deep ultraviolet band is developed to promote the development of related disciplines and industrial technologies.
Drawings
FIG. 1 shows Sr (NH) 2 SO 3 ) 2 Single crystal X-ray powder diffraction pattern.
FIG. 2 is Sr (NH) 2 SO 3 ) 2 Schematic diagram of the unit cell structure of the crystal.
FIG. 3 is Sr (NH) 2 SO 3 ) 2 The crystal is used as a typical schematic diagram of nonlinear optical effect when the frequency doubling crystal is applied, wherein 1 is a laser, 2 is an incident laser beam, 3 is the single crystal of the 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 scheme of the invention will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
The Sr (NH) obtained in the following examples was measured using a physical Mini-flex 600 powder diffractometer equipped with a Cu target 2 SO 3 ) 2 Characterizing the single crystal; test conditions: room temperature.
Example 1
Preparation of Sr (NH) by constant temperature evaporation reaction 2 SO 3 ) 2 (Single Crystal)
Preparation of Sr (NH) 2 SO 3 ) 2 Raw materials for single crystal: srCO 3 0.74g(0.005mol)
NH 2 SO 3 H 0.97g(0.011mol)
The specific operation steps are as follows: weighing the raw materials according to the dosage in an operation box, uniformly mixing, adding into a 25mL beaker, and adding 3Placing the beaker into a baking oven, slowly heating the baking oven to 60 ℃, and evaporating at constant temperature for 3 days to obtain Sr (NH) with the size of 2.5 multiplied by 1 multiplied by 0.8mm 2 SO 3 ) 2 And (3) single crystals.
Sr (NH) obtained in this example 2 SO 3 ) 2 The X-ray powder diffraction pattern of the single crystal is shown in fig. 1, and the results in the graph indicate that: sr (NH) obtained in the present example 2 SO 3 ) 2 The single crystal is single pure phase and has high purity.
The unit cell structure schematic diagram is shown in figure 2. Obtained Sr (NH) 2 SO 3 ) 2 The single crystal has no symmetry center, belongs to monoclinic system, has a space group of Pc and has a unit cell parameter of α=γ=90°, β= 107.803 (9), z=2; the unit cell volume is +.>
Example 2
Preparation of Sr (NH) by constant temperature evaporation reaction 2 SO 3 ) 2 (Single Crystal)
Preparation of Sr (NH) 2 SO 3 ) 2 Raw materials for single crystal: srCO 3 36.91g(0.25mol)
NH 2 SO 3 H 53.40g(0.55mol)
The specific operation steps are as follows: weighing the raw materials according to the above dosage in an operation box, mixing uniformly, then filling 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 3X 1.2X 1mm 2 SO 3 ) 2 And (3) single crystals.
Example 3
For Sr (NH) obtained in example 2 2 SO 3 ) 2 Doubling of the crystal sampleFrequency test experiments are shown in figure 3.
Sr (NH) obtained in example 2 2 SO 3 ) 2 The crystal was cut, oriented, polished and then placed in position 3 in the apparatus shown in fig. 3. YAG laser is used as an input light source (namely a laser 1) with Q-switched Nd: YAG laser at room temperature, the incident wavelength of an incident laser beam 2 is 1064nm, after the incident laser beam 2 is subjected to crystal post-treatment and optical processing of the single crystal 3 of the embodiment 2, the emergent laser beam 4 is observed to be obviously 532nm frequency-doubled green light output after passing through a filter 5. Sr (NH) 2 SO 3 ) 2 The output intensity (powder doubling effect) of (a) is about 1.2 times that of the equivalent KDP.
Example 4
Unlike example 3, a significant 266nm frequency doubling ultraviolet output was observed with the frequency doubling light of the Q-switched Nd: YAG laser as the input light source at an incident wavelength of 532 nm.
Example 5
Unlike example 3, a frequency-doubled deep ultraviolet output of 177.3nm was observed with a frequency-doubled frequency light of Q-switched Nd: YAG laser as an input light source at an incident wavelength of 355 nm.
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, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (18)
1. Strontium sulfamate Sr (NH) 2 SO 3 ) 2 Use of crystals in optical devices;
said Sr (NH) 2 SO 3 ) 2 The crystal has no symmetry center, belongs to monoclinic system, has a space group of Pc and has a unit cell parameter ofα＝γ＝90°，β＝107.803(9)。
2. The use according to claim 1, wherein,
said Sr (NH) 2 SO 3 ) 2 The number of molecules in the unit cell of the crystal z=2;
and/or the Sr (NH) 2 SO 3 ) 2 The unit cell volume of the crystal is
And/or the Sr (NH) 2 SO 3 ) 2 The powder frequency doubling effect of the crystal is KH 2 PO 4 1.2 times of (2);
and/or the Sr (NH) 2 SO 3 ) 2 The ultraviolet absorption edge of the crystal is shorter than 200nm;
and/or the Sr (NH) 2 SO 3 ) 2 The crystal is colorless transparent crystal.
3. The use according to claim 2, wherein,
the volume of the crystal is more than 2.0mm 3 。
4. Use according to claim 1, characterized in that Sr (NH 2 SO 3 ) 2 The preparation method of the crystal comprises the steps of mixing SrCO 3 And NH 2 SO 3 H, reacting to obtain the strontium sulfamate compound.
5. The use according to claim 4 wherein the SrCO 3 And NH 2 SO 3 The molar ratio of H is 1 (2-2.5);
and/or the reaction is carried out in a solvent selected from an organic solvent or an inorganic solvent;
and/or the volume ratio of the total mass of the raw materials to the solvent is (50-80) g/100 mL;
and/or, the temperature of the reaction is 40-100 ℃;
and/or the reaction time is 1-10 days;
and/or, the preparation method further comprises: and collecting the strontium sulfamate compound from the reaction solution after the reaction.
6. The use according to claim 5, wherein the SrCO 3 And NH 2 SO 3 The molar ratio of H is 1 (2.1-2.4);
and/or the solvent is an inorganic solvent;
and/or the volume ratio of the total mass of the raw materials to the solvent is (50-60) g/100 mL;
and/or, the temperature of the reaction is 50-90 ℃;
and/or the reaction time is 3-7 days.
7. The use according to claim 6, wherein,
the solvent is water.
8. The method according to claim 5, wherein the Sr (NH) 2 SO 3 ) 2 And (5) a crystal.
9. The use according to claim 8, wherein,
the evaporating temperature is 50-70 ℃;
and/or the evaporation time is 2-10 days;
and/or the Sr (NH) 2 SO 3 ) 2 The volume of the crystal is more than 2.0mm 3 。
10. The use according to claim 9, wherein,
the evaporating temperature is 55-65 ℃;
and/or the evaporation time is 2.5-8 days.
11. The use according to claim 1, wherein,
the device is used for frequency conversion of laser output of a laser, harmonic generator of ultraviolet region, optical parameter and amplifying device or optical waveguide device.
12. The use according to claim 11, wherein,
which is used to generate 2, 3, 4, 5 or 6 times harmonic light output for a laser beam with a wavelength of 1.064 μm;
and/or it is used for optical parametric and amplifying devices from the infrared to the ultraviolet region.
13. An optical device comprising the strontium sulfamate crystal of any of claims 1-3.
14. The optical device of claim 13, wherein,
the optical device is a laser, a harmonic generator, an optical parameter and amplifying device or an optical waveguide device.
15. The optical device of claim 14, wherein the optical device is a laser.
16. The optical device of claim 15, wherein the laser is an all-solid-state laser.
17. An all-solid-state laser, characterized in that it contains Sr (NH) 2 SO 3 ) 2 And (5) a crystal.
18. An all solid state laser as claimed in claim 17 wherein,
the all-solid-state laser is an all-solid-state deep ultraviolet laser.
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Citations (5)
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|---|---|---|---|---|
| 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 |
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- 2020-08-11 CN CN202010803194.4A patent/CN114074928B/en active Active
Patent Citations (5)
| 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)
| Title |
|---|
| Vibrational modes of strontium sulphamate crystals;M.H.Kuok;Jurnal Fizik Malaysia;第7卷;第152-157页 * |
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