Compound lead chlorate and lead chlorate infrared nonlinear optical crystal, preparation method and use

A non-linear optics, lead chlorate technology, applied in chemical instruments and methods, chloric acid, chlorate, etc., can solve the problem that the research of new frequency conversion crystal needs to be strengthened, and achieves air stability, short reaction time, and preparation method. simple effect

Active Publication Date: 2017-10-17
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Application Information

AI Technical Summary

Problems solved by technology

In the book "Nonlinear Optical Crystal Materials Science" published by Science Press in 2003, it was clearly stated that "in the entire spectral band of nonlinear optics, nonlinear optical crystals in the infrared band are a weak link. Therefore, in this band Research on new frequency conversion crystals needs to be strengthened”

Method used

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  • Compound lead chlorate and lead chlorate infrared nonlinear optical crystal, preparation method and use
  • Compound lead chlorate and lead chlorate infrared nonlinear optical crystal, preparation method and use
  • Compound lead chlorate and lead chlorate infrared nonlinear optical crystal, preparation method and use

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Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1 (adopting melt method)

[0036] Synthetic lead chlorate (Pb 2.14 OCl 2.28 ) compounds:

[0037] Using the solid phase reaction method, according to the chemical equation: 1.14PbCl 2 +PbO→Pb 2.14 OCl 2.28 Synthesis of lead chlorate compounds:

[0038] PbCl 2, PbO was put into a mortar with a stoichiometric ratio of 1.14:1, mixed and carefully ground, then put into a corundum crucible with an opening of Φ400mm×400mm, compacted, put into a muffle furnace, and slowly heated up to 300°C, Constant temperature for 24 hours, take out the crucible after cooling, the sample is relatively loose at this time, then take out the sample and grind it evenly, then put it in the crucible, keep the temperature in the muffle furnace at 430°C for another 48 hours, take it out, put it in the mortar Smash and grind to get the lead chlorate compound, carry out X-ray analysis to this product, the obtained X-ray spectrogram is consistent with that of Pb 2.14 OCl 2.28 The X-...

Embodiment 2

[0046] According to the reaction formula 1.14PbCl 2 +Pb(CO 3 ) 2 →Pb 2.14 OCl 2.28 +CO 2 ↑ Synthesis of Pb 2.14 OCl 2.28 Compound, specific operation steps are carried out according to embodiment 1;

[0047] Preparation of Pb by Pulling Method 2.14 OCl 2.28 Crystal:

[0048] a, the synthesized Pb 2.14 OCl 2.28 Put the compound into an open platinum crucible of Φ100mm×100mm, heat it to a temperature of 600°C, and keep the temperature constant for 5 hours to obtain a mixed melt of lead chlorate;

[0049] b. Preparation of lead chlorate seed crystals: Slowly lower the mixed melt or mixed melt obtained in step a to room temperature at a rate of 0.5° C. / h, and spontaneously crystallize to obtain lead chlorate seed crystals;

[0050] C, the crucible that fills the mixed melt that step a makes is placed in the crystal growth furnace, the Pb that the seed crystal that step b obtains is cut along the c-axis 2.14 OCl 2.28 The seed crystal is fixed on the lower end of the s...

Embodiment 3

[0053] Embodiment 3 (adopting melt method)

[0054] According to the reaction formula 1.14PbCl 2 +PbC 2 0 4 →Pb 2.14 OCl 2.28 +CO 2 ↑+CO↑ Synthesis of Pb 2.14 OCl 2.28 Compound, specific operation steps are carried out according to embodiment 1;

[0055] Preparation of Pb by Kyropoulos method 2.14 OCl 2.28 Crystal:

[0056] a, the synthesized Pb 2.14 OCl 2.28 The compound is put into a Φ100mm×100mm open platinum crucible and heated to melt, heated to a temperature of 600°C, and kept at a constant temperature for 25 hours to obtain a mixed melt of lead chlorate;

[0057] b. Preparation of lead chlorate seed crystals: Slowly lower the mixed melt obtained in step a to room temperature at a rate of 2° C. / h, and spontaneously crystallize to obtain lead chlorate seed crystals;

[0058] C, the crucible that fills the mixed melt that step a makes is placed in the crystal growth furnace, the Pb that the seed crystal that step b obtains is cut along the c-axis 2.14 OCl 2....

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Abstract

The present invention relates to a compound lead chlorate and infrared nonlinear optical crystal of lead chlorate and its preparation method and application. The chemical formula of the compound is Pb2.14OCl2.28, the molecular weight is 545.802, and it is made by solid-state reaction method. The chemical formula of the compound crystal is It is Pb2.14OCl2.28, molecular weight 545.802, no symmetry center, belongs to orthorhombic crystal system, space group Fmm2, unit cell parameters are a=5.829(3) Å,b=16.056(6) Å,c=35.528(15 ) Å, using the compound melt method to grow crystals or adding a cosolvent to grow crystals, the crystal material obtained by the present invention has a strong phase-matching frequency doubling effect (SHG), and the Kurtz powder frequency doubling test results show that its powder doubling The frequency effect is 4 times that of potassium dihydrogen phosphate (KDP), which can achieve phase matching, and the transmission band is 0.34-7μm; the laser damage threshold is 10 times that of the current commercial infrared nonlinear optical crystal material AgGaS2; It does not contain crystal water, is stable to air, and has good thermal stability. It has important application value in laser frequency conversion, electro-optic modulation, photorefractive information processing and other fields.

Description

technical field [0001] The present invention relates to a kind of compound lead chlorate and infrared nonlinear optical crystal of lead chlorate and preparation method and application, and the chemical formula of this compound is Pb 2.14 OCl 2.28 . Background technique [0002] Nonlinear optical effects originate from the interaction between laser and medium. When the laser propagates in a medium with non-zero second-order polarizability, nonlinear optical effects such as frequency doubling, sum frequency, difference frequency, and optical parametric amplification will occur. Using the second-order nonlinear optical effect of crystals, nonlinear optical devices such as second harmonic generators, frequency converters, and optical parametric oscillators can be made. In many fields, such as laser technology, atmospheric monitoring, national defense and military, etc., All have important application value. Inorganic nonlinear optical materials play a dominant role in the pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B11/14C30B29/22C30B11/00C30B15/00C30B17/00
Inventor 潘世烈张辉张敏
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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