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Lead strontium silicate compound and preparation method thereof, lead strontium silicate non-linear optical crystal and preparation method and application thereof

A technology of nonlinear optics and compounds, applied in chemical instruments and methods, crystal growth, lasers, etc., can solve problems such as limited commercial applications, deliquescent crystals, and serious layered growth habits

Active Publication Date: 2019-11-05
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to grow large KBBF single crystals due to its hierarchical growth habit, which limits its further commercial application
Although the crystal growth technology of these materials has become increasingly mature, there are still obvious shortcomings: such as crystal deliquescence, long growth cycle, serious layered growth habit and expensive price, etc.

Method used

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  • Lead strontium silicate compound and preparation method thereof, lead strontium silicate non-linear optical crystal and preparation method and application thereof
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  • Lead strontium silicate compound and preparation method thereof, lead strontium silicate non-linear optical crystal and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] According to the reaction formula: PbO+SrCO 3 +SiO2 2 →PbSrSiO 4 +CO 2 ↑Synthetic compound PbSrSiO 4 :

[0046] PbO, SrCO 3 , SiO 2 Weigh it into a mortar with a molar ratio of 1:1:1, mix and grind it carefully, then put it into a corundum crucible with an opening of Φ100mm×100mm, put it into a muffle furnace, slowly raise the temperature to 300°C, and keep the temperature constant for 24 hours. Cool to room temperature, take it out and put it into the muffle furnace after the second grinding, then raise the temperature to 750°C, keep the temperature for 24 hours, cool to room temperature, take it out and put it into the muffle furnace after the third grinding, and then heat it at 750°C Keep the temperature for 48 hours, take out the compound lead strontium silicate single-phase polycrystalline powder obtained by grinding, and carry out X-ray analysis on the product, and the obtained X-ray spectrum is consistent with that of lead strontium silicate PbSrSiO 4 The ...

Embodiment 2

[0053] According to the reaction formula: 2Pb(OH) 2 +2Sr(NO 3 ) 2 +2SiO 2 →2PbSrSiO 4 +4NO 2 ↑+2H 2 O↑+O 2 ↑Synthetic compound PbSrSiO 4 :

[0054] Pb(OH) 2 , Sr(NO 3 ) 2 , SiO 2 Weigh the raw materials directly according to the molar ratio of 1:1:1, and combine the weighed raw materials with the flux SrF 2 -PbF 2 Mixed at a molar ratio of 1:4, where SrF 2 with PbF 2 The molar ratio is 3:5, put it into an open platinum crucible of Φ80mm×80mm, heat up to a temperature of 800°C, and keep the temperature at a constant temperature for 60 hours to obtain a mixed melt, which is cooled to a temperature of 650°C;

[0055] Slowly cool down to room temperature at a rate of 1.5°C / h, and spontaneously crystallize to obtain lead strontium silicate seed crystals;

[0056] PbSrSiO will be obtained 4 The seed crystal is fixed on the seed crystal rod, and the seed crystal is lowered from the top of the crystal growth furnace. The seed crystal is preheated on the surface of the...

Embodiment 3

[0060] According to the reaction formula: 4) PbCl 2 +SrCO 3 +SiO2 2 →PbSrSiO 4 +CO↑+Cl 2 ↑Synthetic compound PbSrSiO 4 :

[0061] PbCl 2 , SrCO 3 , SiO 2 Weigh the raw materials directly with a molar ratio of 1:1:1, and mix the weighed raw materials with the flux LiF-PbO at a molar ratio of 1:3, where the molar ratio of LiF to PbO is 3:1, and put it into a Φ80mm× In a platinum crucible with an opening of 80mm, the temperature was raised to 780°C, and the temperature was kept constant for 60 hours to obtain a mixed melt, and then lowered to a temperature of 620°C;

[0062] Slowly cool down to room temperature at a rate of 3.5°C / h, and spontaneously crystallize to obtain lead strontium silicate seed crystals;

[0063] PbSrSiO will be obtained 4 The seed crystal is fixed on the seed crystal rod, and the seed crystal is lowered from the top of the crystal growth furnace. The seed crystal is preheated on the surface of the mixed melt for 15 minutes, and immersed in the li...

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Abstract

The invention relates to a lead strontium silicate compound and a preparation method thereof, a lead strontium silicate non-linear optical crystal and a preparation method and application thereof. Thechemical formulas of the lead strontium silicate compound and non-linear optical crystal are both PbSrSiO4, the crystal belongs to an orthorhombic system, the space group is P212121, the molecular weight according crystal cell parameters is 338.9, and the powder frequency doubling effect of the compound is about 2 times KDP (KH2PO4). The lead strontium silicate compound is synthesized by means ofa solid phase reaction method, and the lead strontium silicate non-linear optical crystal is obtained by means of a high-temperature solid phase method. The lead strontium silicate non-linear opticalcrystal is high in mechanical hardness and easy to cut, polish, process and preserve and is widely used in preparation of nonlinear optical devices such as frequency doubling generators, upper frequency converters, lower frequency converters and optical parametric oscillators.

Description

technical field [0001] The present invention relates to the chemical formula PbSrSiO 4 The compound lead-strontium silicate nonlinear optical crystal, the preparation method of the crystal and the nonlinear optical device fabricated by using the crystal. Background technique [0002] Ultraviolet (UV) or deep ultraviolet (DUV) nonlinear optics (NLO) materials play an important role in laser frequency conversion, lithography, semiconductor lithography, etc. Due to their ability to generate coherent UV or DUV light over the past few decades, some UV and DUV NLO crystals, including β-BaB 2 o 4 (BBO), LiB 3 o 5 (LBO), CsB 3 o 5 (CBO), CsLiB 6 o 10 (CLBO), KBe 2 BO 3 f 2 (KBBF),K 3 B 6 o 10 Cl(KBOC),Ba 4 B 11 o 20 F(BOBF), so far only KBBF can do this by direct second harmonic generation of DUV coherent light. However, it is difficult to grow large KBBF single crystals due to its hierarchical growth habit, which limits its further commercial applications. Althou...

Claims

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Application Information

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IPC IPC(8): C30B29/34C30B11/00H01S3/16
CPCC30B11/00C30B29/34H01S3/1655
Inventor 吴红萍姜姝彤俞洪伟
Owner TIANJIN UNIVERSITY OF TECHNOLOGY