CN110306240B - Non-linear optical crystal of sodium potassium iodate and its preparation method and use - Google Patents

Non-linear optical crystal of sodium potassium iodate and its preparation method and use Download PDF

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CN110306240B
CN110306240B CN201910681259.XA CN201910681259A CN110306240B CN 110306240 B CN110306240 B CN 110306240B CN 201910681259 A CN201910681259 A CN 201910681259A CN 110306240 B CN110306240 B CN 110306240B
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潘世烈
吐沙姑·阿不都吾甫
张敏
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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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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    • C—CHEMISTRY; METALLURGY
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    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
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Abstract

The invention relates to a potassium sodium iodate nonlinear optical crystal, a preparation method and application thereof, wherein the chemical formula of the crystal is K2Na(IO3)2(I3O8) Molecular weight of 959.69, belonging to monoclinic system, space group of Pc, unit cell parameters of a =11.4483(6) Å, b =8.1332(5) Å, c =7.8077(4) Å, α =90 °, β =90.239 °, γ =90 °, V =726.98(7) Å3. The wide light transmission range is provided, the ultraviolet transmission cut-off edge is 290n, the optical band gap is 4.27eV, and the nonlinear optical effect is about 7.6 times of KDP. The crystal adopts a hydrothermal method, can obtain a millimeter-grade transparent sodium potassium iodate nonlinear optical crystal by a programmed cooling or constant temperature method, has the advantages of simple operation, low cost, inorganic reagents used as raw materials, short growth period, stable physicochemical properties and the like, and can be widely applied to nonlinear optical devices such as frequency doubling conversion, optical parametric oscillators and the like.

Description

Non-linear optical crystal of sodium potassium iodate and its preparation method and use
Technical Field
The invention relates to an iodate nonlinear optical crystal and a preparation method and application thereof, wherein potassium sodium iodate belongs to the field of inorganic chemistry, and also belongs to the fields of crystallography, material science and optics.
Background
The development of nonlinear optics and its crystal materials is closely related to the development of laser technology. The method has important application value in high-tech fields such as laser frequency conversion, photoelectric communication, optical information processing, integrated circuits and the like. In the laser technology, the laser wave band obtained by directly utilizing the laser crystal is limited, the nonlinear optical crystal is utilized for frequency conversion, and the laser output by the all-solid-state laser can be converted into the laser with a new wave band, so that the application range of the laser is greatly expanded, and the market economic value is improved. Such nonlinear optical materials are also the material basis of the optoelectronics industry, and are important pillars for the development of the fields of solid-state laser technology, optical communication, information processing, and the like.
The second-order nonlinear optical crystal which is currently put into practical use comprises KH2PO4(KDP)，KTiOPO4(KTP)，LiNbO3(LNO)，BaTiO3(BTO)，α-LiIO3，KIO3And the like. With the development of laser technology and the emergence of tunable lasers, nonlinear optical devices develop rapidly, and laser frequency doubling, frequency mixing, parametric oscillation and amplification are achieved; electro-optical modulation, deflection, Q-switching, and photorefractive devices, etc. occur sequentially. The research and application mentioned above put more and higher requirements on the physical and chemical properties of the nonlinear optical material, and also promote the rapid development of the nonlinear optical material. The inorganic groups giving rise to noncardial structures predominantly comprise BO3 3-、PO4 3-And ions containing lone pairs of electrons (e.g. I (V), Se (IV), Bi (III), Pb (II), Te (IV), etc.) and distorted octahedral coordination d0Electron configuration transition metal ions (e.g., Ti (IV), V (V), Nb (V), Ta (V), Mo (VI), W (VI), etc.). Among them, the metal iodate nonlinear optical crystal is widely noticed for its excellent optical properties. Studies have shown that crystals of nonlinear optical properties are readily obtained if a non-centrosymmetric coordination environment is formed in the compound. Because the metal iodate crystal has stronger frequency doubling effect, wider transmission waveband, higher thermal stability and optical damage threshold, the metal iodate crystal plays a very important role in the field of second-order nonlinear optical crystal materials. In addition, it is worth mentioning IO3 -，IO4 3-The isoradicals have large microscopic nonlinear optical coefficients, which are due in large part to the lone pair of electrons they containThree relatively close energy levels are provided, making it more advantageous to increase the nonlinear optical coefficient.
Sodium potassium iodate (K)2Na(IO3)2(I3O8) The crystal is a novel nonlinear optical crystal material, and the invention researches the potassium sodium iodate crystal with high optical quality. The test shows that: the second-order nonlinear optical coefficient of the crystal is equivalent to 7.6 times KDP, the ultraviolet transmission cut-off edge is 290nm, and the optical band gap is 4.27 eV. And other physical, chemical, thermal and mechanical properties of the crystal are ideal. Therefore, the sodium potassium iodate crystal is expected to be used as a novel nonlinear optical crystal material to obtain corresponding variable frequency laser output with higher efficiency, thereby obtaining practical application.
Disclosure of Invention
The invention aims to provide a potassium sodium iodate nonlinear optical crystal with a chemical formula of K2Na(IO3)2(I3O8) Molecular weight of 959.69, belonging to monoclinic system, space group of Pc, unit cell parameter of
Figure BDA0002144817150000021
Figure BDA0002144817150000022
α＝90°，β＝90.239°，γ＝90°，
Figure BDA0002144817150000023
Figure BDA0002144817150000024
Another object of the present invention is to provide a method for preparing and growing a nonlinear optical crystal of sodium potassium iodate by using a hydrothermal method, which is simple and convenient to operate.
It is another object of the present invention to provide the use of non-linear optical crystals of potassium sodium iodate for the preparation of visible mid-and far-infrared laser frequency output.
The invention also aims to provide the application of the potassium sodium iodate nonlinear optical crystal in preparing a frequency doubling generator and an optical parametric oscillator.
The invention relates to a potassium sodium iodate nonlinear optical crystal, the chemical formula of which is K2Na(IO3)2(I3O8) Molecular weight of 959.69, belonging to monoclinic system, space group of Pc, unit cell parameter of
Figure BDA0002144817150000025
Figure BDA0002144817150000026
α＝90°，β＝90.239°，γ＝90°，
Figure BDA0002144817150000027
The preparation method of the potassium sodium iodate nonlinear optical crystal adopts a hydrothermal method to grow the crystal, and the specific operation is carried out according to the following steps:
a. the K with the purity of 99.9 percent is added2CO3With HIO of 99.5% purity3And Na2SO4Putting the mixture into a mortar according to the mol ratio of 1.25-3:3-5:2, mixing and fully grinding the mixture, adding 2-4ml of deionized water, stirring the mixture at the temperature of 40-80 ℃ until the mixture is dissolved, and filtering and removing precipitates to obtain a saturated solution of potassium sodium iodate;
b. and (b) pouring 2-4ml of the potassium sodium iodate saturated solution obtained in the step (a) into 23-100ml of a hydrothermal kettle with a polytetrafluoroethylene lining, screwing and sealing the hydrothermal kettle, putting the hydrothermal kettle into a box-type resistance furnace, heating to 180 ℃ and 220 ℃ at a heating rate of 20-60 ℃/h, keeping the temperature for 3-15 days, cooling to room temperature at a cooling rate of 1-10 ℃/h, and opening the hydrothermal kettle to obtain the potassium sodium iodate nonlinear optical crystal.
The potassium sodium iodate nonlinear optical crystal is used for preparing visible middle and far infrared laser frequency output.
The potassium sodium iodate nonlinear optical crystal is used for preparing a frequency doubling generator and an optical parametric oscillator.
The molecular formula of the potassium sodium iodate nonlinear optical crystal is K2Na(IO3)2(I3O8) The ultraviolet transmission cut-off edge is 290nm, the nonlinear optical effect is about 7.6 times of KDP, and the space group is Pc. The crystal is simple to prepare and short in growth period.
The preparation method of the potassium sodium iodate nonlinear optical crystal is a hydrothermal method, namely, the initial raw materials are mixed according to a ratio and then are placed in a high-pressure reaction kettle, and the millimeter-grade transparent potassium sodium iodate nonlinear optical crystal can be obtained through constant temperature and cooling rate within a certain temperature range.
In the invention K2CO3，HIO3And Na2SO4The compounds can adopt commercially available reagents and raw materials, and the crystal is extremely easy to grow and is transparent, so that the method has the advantages of simple operation, high growth speed, low cost, easy obtainment of large-size crystals and the like.
The invention relates to a sodium potassium iodate nonlinear optical crystal prepared by the method, and application of the crystal in preparing a frequency doubling generator, an optical parametric oscillator or a lens.
Drawings
FIG. 1 is a powder X-ray diffraction pattern of the present invention;
FIG. 2 is a crystal structure of the present invention;
fig. 3 is a schematic diagram of the operation of the nonlinear optical device according to the present invention, which includes (1) a laser, (2) an all-focusing lens, (3) a sodium potassium iodate nonlinear optical crystal, (4) a beam splitter prism, and (5) a filter, where ω is the frequency of the refracted light equal to or 2 times the frequency of the incident light.
Detailed Description
The invention is described in detail below with reference to the following figures and examples:
example 1
Growing potassium sodium iodate crystals by a hydrothermal method:
the K with the purity of 99.9 percent is added according to the mol ratio of 1.25:3:22CO3With HIO of 99.5% purity3And Na2SO4Mixing in mortar, grinding, dissolving in 2ml deionized water, stirring at 40 deg.C until the mixture is dissolved, filtering to remove precipitate to obtain potassium iodateA sodium saturated solution;
pouring the obtained saturated solution of potassium sodium iodate into a 23ml hydrothermal kettle with a polytetrafluoroethylene lining, screwing and sealing the hydrothermal kettle, putting the hydrothermal kettle into a box-type resistance furnace, heating to 180 ℃ at a heating rate of 20 ℃/h, keeping the temperature for 3 days, cooling to room temperature at a cooling rate of 1 ℃/h, and opening the hydrothermal kettle to obtain the 3mm x 2mm x 1mm potassium sodium iodate nonlinear optical crystal.
Example 2
Growing potassium sodium iodate crystals by a hydrothermal method:
the K with the purity of 99.9 percent is added according to the mol ratio of 1.25:4:22CO3With HIO of 99.5% purity3And Na2SO4Mixing and fully grinding the mixture in a mortar, fully dissolving the mixture by using 3ml of deionized water, stirring the mixture at the temperature of 60 ℃ until the mixture is dissolved, and filtering and removing precipitates to obtain a saturated solution of potassium sodium iodate;
pouring the obtained saturated solution into a 50ml hydrothermal kettle with a polytetrafluoroethylene lining, screwing and sealing the hydrothermal kettle, putting the hydrothermal kettle into a box-type resistance furnace, heating to 200 ℃ at the temperature rise rate of 30 ℃/h, keeping the temperature for 3 days, cooling to room temperature at the temperature drop rate of 10 ℃/h, and opening the hydrothermal kettle to obtain the potassium sodium iodate nonlinear optical crystal with the size of 3mm multiplied by 1 mm.
Example 3
Growing potassium sodium iodate crystals by a hydrothermal method:
the K with the purity of 99.9 percent is added according to the mol ratio of 2:4:22CO3With HIO of 99.5% purity3And Na2SO4Mixing and fully grinding the mixture in a mortar, fully dissolving the mixture by using 4ml of deionized water, stirring the mixture at the temperature of 80 ℃ until the mixture is dissolved, and filtering and removing precipitates to obtain a saturated solution of potassium sodium iodate;
pouring the obtained saturated solution of potassium sodium iodate into a 100ml hydrothermal kettle with a polytetrafluoroethylene lining, screwing and sealing the hydrothermal kettle, putting the hydrothermal kettle into a box-type resistance furnace, heating to 220 ℃ at a heating rate of 40 ℃/h, keeping the temperature for 15 days, cooling to room temperature at a cooling rate of 10 ℃/h, and opening the hydrothermal kettle to obtain the 1mm x 2mm x 3mm potassium sodium iodate nonlinear optical crystal.
Example 4
Growing potassium sodium iodate crystals by a hydrothermal method:
the K with the purity of 99.9 percent is added according to the mol ratio of 2:5:22CO3With HIO of 99.5% purity3And Na2SO4Mixing and fully grinding the mixture in a mortar, fully dissolving the mixture by using 3ml of deionized water, stirring the mixture at the temperature of 80 ℃ until the mixture is dissolved, and filtering and removing precipitates to obtain a saturated solution of potassium sodium iodate;
pouring the obtained saturated solution of potassium sodium iodate into a 100ml hydrothermal kettle with a polytetrafluoroethylene lining, screwing and sealing the hydrothermal kettle, putting the hydrothermal kettle into a box-type resistance furnace, heating to 220 ℃ at a heating rate of 60 ℃/h, keeping the temperature for 10 days, cooling to room temperature at a cooling rate of 10 ℃/h, and opening the hydrothermal kettle to obtain the 1mm x 5mm x 3mm potassium sodium iodate nonlinear optical crystal.
Example 5
Any of the sodium potassium iodate nonlinear optical crystals obtained in examples 1-4 was placed at the position 3 as shown in fig. 3, and at room temperature, a 1064nm output of a Q Nd: YAG laser was used as a light source to observe an obvious 532nm frequency-doubled green light output with an output intensity of about 7.6 times that of KDP under the same conditions, as shown in fig. 3, a 1064nm wavelength infrared beam emitted from the Q Nd: YAG laser 1 was incident on the sodium potassium iodate nonlinear optical crystal through a hololens 2 to generate a 532nm wavelength green frequency-doubled light, and the emergent beam 4 contained a 1064nm wavelength infrared light and a 532nm green light, which was filtered by a filter 5 to obtain a 532nm wavelength frequency-doubled light.

Claims (4)

1. A non-linear optical crystal of sodium potassium iodate is characterized by that its chemical formula is K2Na(IO3)2(I3O8) Molecular weight of 959.69, belonging to monoclinic system, space group of Pc, unit cell parameters of a =11.4483(6) Å, b =8.1332(5) Å, c =7.8077(4) Å, α =90 °, β =90.239 °, γ =90 °, V =726.98(7) Å3。
2. The method for preparing the non-linear optical crystal of sodium potassium iodate as defined in claim 1, which is characterized by that it adopts hydrothermal method to grow crystal, and its concrete operation is implemented by the following steps:
a. the K with the purity of 99.9 percent is added2CO3With HIO of 99.5% purity3And Na2SO4Putting the mixture into a mortar according to the mol ratio of 1.25-3:3-5:2, mixing and fully grinding the mixture, adding 2-4ml of deionized water, stirring the mixture at the temperature of 40-80 ℃ until the mixture is dissolved, and filtering and removing precipitates to obtain a saturated solution of potassium sodium iodate;
b. and (b) pouring 2-4ml of the potassium sodium iodate saturated solution obtained in the step (a) into 23-100ml of a hydrothermal kettle with a polytetrafluoroethylene lining, screwing and sealing the hydrothermal kettle, putting the hydrothermal kettle into a box-type resistance furnace, heating to 180 ℃ and 220 ℃ at a heating rate of 20-60 ℃/h, keeping the temperature for 3-15 days, cooling to room temperature at a cooling rate of 1-10 ℃/h, and opening the hydrothermal kettle to obtain the potassium sodium iodate nonlinear optical crystal.
3. Use of the potassium sodium iodate nonlinear optical crystal of claim 1 in the preparation of visible mid-far infrared laser frequency output.
4. Use of the potassium sodium iodate nonlinear optical crystal according to claim 1 in the preparation of frequency doubling generators, optical parametric oscillators.
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