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Method for growing large-size lithium lead phosphate single crystals through hydrothermal method

A technology of lead lithium phosphate and hydrothermal method, which is applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., can solve the problem that the nonlinear material of lead lithium phosphate has not been effectively applied and developed, and affects the photoelectric performance of the material and the optical quality of the crystal. Poor and other problems, to achieve the effect of small stress, good compatibility and high utilization rate of raw materials

Inactive Publication Date: 2017-12-15
桂林百锐光电技术有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The methods for preparing lithium lead phosphate materials in the prior art mainly include solid phase synthesis, melt method and co-solvent method. The solid-phase synthesis method is suitable for micro-nano powders. Although the melt method and co-solvent can synthesize larger crystal However, other impurities will inevitably be introduced, which will eventually affect the photoelectric properties of the material.
At present, the main methods for growing lithium lead phosphate crystals are pulling method, crucible drop method and co-solvent method, but the crystals obtained by the above methods are of poor optical quality (high impurity content, high color center and high dislocation density), and the size is uneven. Small, so that lithium lead phosphate nonlinear materials have not been effectively applied and developed

Method used

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  • Method for growing large-size lithium lead phosphate single crystals through hydrothermal method
  • Method for growing large-size lithium lead phosphate single crystals through hydrothermal method
  • Method for growing large-size lithium lead phosphate single crystals through hydrothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Take LiH 2 PO 4 Use distilled water to make LiH with a concentration of 3mol / L 2 PO 4 The solution is used as a mineralizer for standby;

[0025] 2) Weigh lead chloride (PbCl 2 )56g, lithium dihydrogen phosphate (LiH 2 PO 4 ) 21g, ball milled and mixed evenly as a hydrothermal reactant, placed at the bottom of the gold bushing tube (reaction chamber Φ35mm) of the autoclave;

[0026] 3) Add 154mL of mineralizer into the gold bushing tube (the filling degree of mineralizer is 65%, the solid-liquid ratio of hydrothermal reactant and mineralizer is 0.5g:1mL), and hang a A gold wire is used to weld and seal the gold bushing tube, and then put it into an autoclave with a matching caliber;

[0027] 4) Fill 65% volume of deionized water between the outer wall of the gold liner pipe and the interlayer of the inner wall of the autoclave, and seal the autoclave;

[0028] 5) Put the sealed autoclave into a two-stage heating resistance furnace, set the average temperature...

Embodiment 2

[0034] 1) Take LiH 2 PO4 Use distilled water to make LiH with a concentration of 5mol / L 2 PO 4 The solution is used as a mineralizer for standby;

[0035] 2) Weigh lead fluoride (PbF 2 ) 100g, lithium dihydrogen phosphate (LiH 2 PO 4 ) 42.4g, ball milled and mixed uniformly as a hydrothermal reactant, placed at the bottom of the gold bushing tube (reaction chamber Φ35mm) of the autoclave;

[0036] 3) Add 142.4mL of mineralizer into the gold bushing tube (the filling degree of mineralizer is 70%, the solid-liquid ratio of hydrothermal reactant and mineralizer is 1g:1mL), and hang a A gold wire, hang 2 lead-lithium phosphate monochips (respectively (001) and (011) directions) on the gold wire, weld and seal the gold bushing tube, and then put it into an autoclave with a matching caliber;

[0037] 4) Fill 70% volume of deionized water between the outer wall of the gold liner tube and the interlayer of the inner wall of the autoclave, and seal the autoclave;

[0038] 5) Put...

Embodiment 3

[0040] 1) Take LiH 2 PO 4 Use distilled water to make LiH with a concentration of 1mol / L 2 PO 4 The solution is used as a mineralizer for standby;

[0041] 2) Weigh lead nitrate (PbSO 4 ) 46g, lead phosphate (Pb 3 (PO 4 ) 2 ) 121.7g, lithium dihydrogen phosphate (LiH 2 PO 4 ) 31.5g, ball milled and mixed evenly as a hydrothermal reactant, placed at the bottom of the gold bushing tube (reaction chamber Φ30mm) of the autoclave;

[0042] 3) Add 132.8mL of mineralizer to the gold bushing tube (the filling degree of mineralizer is 80%, the solid-liquid ratio of hydrothermal reactant and mineralizer is 1.5g: 1mL), and hang it on the top of the gold bushing tube A gold wire, two primary crystals of lithium lead phosphate are hung on the gold wire, the gold bushing tube is welded and sealed, and then put into an autoclave with a matching caliber;

[0043] 4) Fill 80% volume of deionized water between the outer wall of the gold liner pipe and the interlayer of the inner wall ...

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Abstract

The invention discloses a method for growing large-size lithium lead phosphate single crystals through a hydrothermal method. The method includes the steps that a lead source and lithium dihydrogen phosphate are put into an autoclave as hydrothermal reactants, a lithium dihydrogen phosphate solution and / or a dilithium hydrogen phosphate solution with the lithium ion concentration of 1-5 mol / L serve / serves as a mineralizer, and a temperature-difference hydrothermal method is adopted to make the hydrothermal reactants subjected to a combination reaction to obtain the lithium lead phosphate single crystals after growth. According to the method, the lead source and lithium dihydrogen phosphate are directly subjected to the combination reaction in the autoclave under the temperature-difference hydrothermal condition to obtain the lithium lead phosphate single crystals after growth, and the basic reaction materials do not need to be pressed or sintered, so that the process is simpler; besides, the lithium dihydrogen phosphate solution and / or the dilithium hydrogen phosphate solution are / is adopted as the mineralizer, other impurities will not be introduced, the material utilization rate is high, the concentration compatibility of the mineralizer is high, and the large-size lithium lead phosphate single crystals can be obtained.

Description

technical field [0001] The invention relates to a method for preparing a lithium lead phosphate single crystal, in particular to a method for growing a large-sized lithium lead phosphate single crystal by a hydrothermal method. Background technique [0002] Nonlinear optical materials can effectively expand the fixed or limited wavelength range of laser sources, so they play a pivotal role in the fields of high-density optical data storage, color imaging, ultrafine spectral analysis, precise microprocessing, biotechnology, medicine, and photochemistry. [0003] In the past few decades, researchers at home and abroad have reported a large number of high-performance nonlinear materials, such as: β-BaB 2 o 4 (BBO), LiB 3 o 5 (LBO), CsB 3 o 5 (CBO), CsLiB 6 o 10 (CLBO) 5 、KH 2 PO 4 (KDP), KTiOPO 4 (KTP) and KBe 2 BO 3 f 2 (KBBF) etc. However, these materials have their own shortcomings. It is still a challenge to design and synthesize new nonlinear materials suita...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B7/14C30B29/14
CPCC30B7/10C30B7/14C30B29/14
Inventor 任孟德王金亮卢福华何小玲周海涛左艳彬吴文渊张昌龙李东平覃世杰胡乔帆
Owner 桂林百锐光电技术有限公司
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