Method for preparing lead fluoroborate single crystal by microwave hydrothermal method

A lead fluoroborate and microwave hydrothermal technology, applied in the field of material science, can solve the problems of difficult control of the process, high price, and long experiment cycle, and achieve excellent nonlinear optical performance, low equipment cost, and short experiment cycle.

Inactive Publication Date: 2015-04-15
XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST
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Problems solved by technology

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.
However, the high-temperature solution method to grow crystals requires a long experimental period, complicated operations, difficult selection of flux, difficult control of the process, and poor repeatability.

Method used

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  • Method for preparing lead fluoroborate single crystal by microwave hydrothermal method
  • Method for preparing lead fluoroborate single crystal by microwave hydrothermal method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] a. Analytical pure PbF 2 and H 3 BO 3 Mix at a molar ratio of 1:3, then dissolve in 0.2mol / L hydrofluoric acid, and keep stirring to make a suspension A with a Pb ion concentration of 0.1mol / L;

[0020] b. Add the mineralizer LiF into distilled water and keep stirring to prepare a transparent solution B with a Li ion concentration of 0.4mol / L;

[0021] c. Mix the suspension A obtained in step a with the transparent solution B obtained in step b in a molar ratio of Pb:Li=1:1 and stir evenly, then adjust the pH value of the solution to 9 with analytically pure LiOH, and fully Stir for 30min to obtain solution C;

[0022] d. Place the solution C obtained in step c in a hydrothermal reaction kettle, control the filling ratio to 40%, then put it into a temperature-pressure dual-control microwave hydrothermal reaction instrument, select the temperature control mode, and the temperature control temperature is 140°C. The reaction time is 1h, and the reaction is naturally co...

Embodiment 2

[0025] a. Analytical pure PbF 2 and H 3 BO 3 Mix at a molar ratio of 1:3, then dissolve in 0.1mol / L hydrofluoric acid, and keep stirring to make a suspension A with a Pb ion concentration of 0.5mol / L;

[0026] b. Add the mineralizer LiF into distilled water, and keep stirring to prepare a transparent solution B with a Li ion concentration of 0.1mol / L;

[0027] c. Mix and stir the suspension A obtained in step a and the transparent solution B obtained in step b in a molar ratio of Pb:Li=1:2, then use analytically pure LiOH to adjust the pH value of the solution to 10, and stir again for 60 minutes Obtain solution C;

[0028] d. Place the solution C obtained in step c in a hydrothermal reaction kettle, control the filling ratio to 40%, and then put it into a temperature-pressure dual-control microwave hydrothermal reactor, select the temperature control mode, and the temperature control temperature is 160°C. The reaction time is 2h, and the reaction is naturally cooled to ro...

Embodiment 3

[0031] a. Analytical pure PbF 2 and H 3 BO 3 Mix at a molar ratio of 1:3, then dissolve in 0.6mol / L hydrofluoric acid, and keep stirring to make a suspension A with a Pb ion concentration of 1mol / L;

[0032] b. Add the mineralizer LiF into distilled water, and keep stirring to prepare a transparent solution B with a Li ion concentration of 0.5mol / L;

[0033]c. Mix and stir the suspension A obtained in step a and the transparent solution B obtained in step b in a molar ratio of Pb:Li=1:3, then use analytically pure LiOH to adjust the pH value of the solution to 11, and stir again for 90 minutes Obtain solution C;

[0034] d. Place the solution C obtained in step c in a hydrothermal reactor, control the filling ratio to 50%, and then put it into a temperature-pressure dual-control microwave hydrothermal reactor, select the temperature control mode, and the temperature control temperature is 170 ° C. The time is 3h, naturally cool to room temperature after the reaction finish...

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Abstract

The invention relates to a method for preparing a lead fluoroborate single crystal by a microwave hydrothermal method. The method is a preparation method which can be implemented by one step in a liquid phase and used for growing lead fluoroborate nonlinear optical crystals by the microwave hydrothermal method by adoption of the microwave hydrothermal method and by use of a microwave quick and efficient heating mode. The lead fluoroborate single crystal prepared by the method is excellent in nonlinear optical performance; the powder frequency-doubled effect is four times better than that of KDP (KH2PO<-4>); the stop edge of an ultraviolet region is about 195nm. Furthermore, the lead fluoroborate single crystal prepared by the microwave hydrothermal method is complete in crystal form and uniform in size, is easy to cut, polish and store and can be widely applied to the preparation of nonlinear optical devices such as a frequency doubling generator, an upper or lower frequency doubling converter and an optical parameter amplifier. The method disclosed by the invention has the characteristics that the raw materials are readily available, the equipment cost is low, the operation is simple, and the experiment period is shorter.

Description

technical field [0001] The invention belongs to the field of material science, and in particular relates to a method for preparing a lead fluoroborate single crystal with nonlinear optical crystals. Background technique [0002] Ultraviolet nonlinear optical materials are the key materials for solid-state lasers to generate ultraviolet coherent light. In order to obtain nonlinear optical materials with nonlinear optical properties, the current international method is to introduce nonlinear optical functions that are easy to cause distortion in the structure. Primitives, these primitives mainly contain d 0 , d 10 Electronic structure of transition metal cation polyhedra or metal cation polyhedra containing lone electron pairs. However, these structural motifs often redshift the UV cut-off edge of the material, making it unsuitable for use in the UV region. The characteristic of borate is that it is beneficial to the transmission of ultraviolet radiation. Many excellent non...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/22C30B7/10
CPCC30B7/10C30B29/22
Inventor 李弘毅潘世烈张芳袁鹿晓泉
Owner XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST
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