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Method for synthesizing LiXSe2 polycrystalline compound and mono-crystal

A compound and single crystal technology, applied in the field of polycrystalline compound and single crystal synthesis, can solve the problems of loss of Se, stoichiometric ratio deviation, etc.

Inactive Publication Date: 2018-07-13
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But the preparation of LiXSe 2 (X=In / Ga / In y Ga 1-y ) crystals also have many problems. Due to the active chemical properties of Li, it is easy to react with quartz crucibles, and a large amount of Se will be lost in the process of synthesis and single crystal preparation.
The current method usually adds a certain excess of Li and Se in advance when synthesizing the polycrystalline material, but the obtained LiXSe 2 (B=In / Ga / In y Ga 1-y ) There is a certain deviation between the composition of the single crystal and its stoichiometric ratio of 1:1:2, and the deviation of Li can reach more than 25%.

Method used

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  • Method for synthesizing LiXSe2 polycrystalline compound and mono-crystal

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Experimental program
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Embodiment 1

[0030] First, soak the inner graphite crucible and the outer quartz crucible with acetone to remove organic impurities, soak them in aqua regia to remove inorganic impurities, then clean them with deionized water, dry them, and put them on the inner wall of the dried quartz crucible Deposit a carbon film. According to the molar ratio of 1:1:2, Li, In and Se are accurately weighed, and an additional 3% of Li and 2% of Se are added, and put into the inner graphite crucible together. After the graphite crucible is covered with a stopper, put it into a carbon-coated quartz crucible, and vacuumize to 5×10 -5 Pa, the quartz crucible was sealed with an oxyhydrogen flame and placed in a rocking furnace. Raise the temperature of the mixing furnace to 180°C at a rate of 30°C / h. At this temperature, Li and Se start to react, reducing the corrosion of the quartz crucible by Li at high temperature and the volatilization of Se. Then the temperature was raised to 230°C at a rate of 10°C / h,...

Embodiment 2

[0032] First, soak the inner PBN crucible and the outer quartz crucible with acetone to remove organic impurities, soak them in aqua regia to remove inorganic impurities, then clean them with deionized water, dry them, and put them on the inner wall of the dried quartz crucible Deposit a carbon film. According to the molar ratio of 1:1:2, the three elements of Li, Ga and Se are accurately weighed, and an additional 2% of Li and 2% of Se are added, and put into the inner PBN crucible together. Put the PBN crucible into the carbon-coated quartz crucible, and evacuate to 5×10 -5 Pa, the quartz crucible was sealed with an oxyhydrogen flame and placed in a rocking furnace. Raise the temperature of the mixing furnace to 180°C at a rate of 40°C / h. At this temperature, Li and Se start to react, reducing the corrosion of the quartz crucible by Li at high temperature and the volatilization of Se. Then the temperature was raised to 220°C at a rate of 5°C / h, and then kept at this temper...

Embodiment 3

[0034] First, soak the inner graphite crucible and the outer quartz crucible with acetone to remove organic impurities, soak them in aqua regia to remove inorganic impurities, then clean them with deionized water, dry them, and put them on the inner wall of the dried quartz crucible Deposit a carbon film. According to the molar ratio of 1:0.5:0.5:2, Li, In, Ga and Se three elements are accurately weighed, and an additional 3% Li and 3% Se are added, and put into the inner graphite crucible together. After the graphite crucible is covered with a stopper, put it into a carbon-coated quartz crucible, and vacuumize to 5×10 -5 Pa, the quartz crucible was sealed with an oxyhydrogen flame and placed in a rocking furnace. Raise the temperature of the mixing furnace to 180°C at a rate of 30°C / h. At this temperature, Li and Se start to react, reducing the corrosion of the quartz crucible by Li at high temperature and the volatilization of Se. Then the temperature was raised to 240°C a...

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Abstract

The invention relates to a preparation method of LiXSe2 polycrystalline compound and mono-crystal. The preparation method comprises the following steps: filling Li, In, Ga and Sa monomers into an inner-layer crucible and a quartz crucible and packaging in vacuum; filling the crucibles into a swinging furnace and carrying out heat preservation and swinging at the temperature above the smelting point of the LiXSe2 compound; then cooling to room temperature. The obtained LiXSe2 (X is equal to In / Ga / InyGa1-y) compound meets a stoichiometric ratio. By controlling the temperature, the Li, In, Ga andSa monomers are subjected to compound reaction at temprature close to smelting points of the Li and the Se under relatively low steam pressure of the Li and the Se, so as to obtain Li2Se, InxSey andGaxSey compounds and the like and fix the chemical activity of the Li and the Se and reduce the loss of Li and Se components; the deviation of the stoichiometric ratio of chemical components of the LiXSe2 mono-crystal (X is equal to In / Ga / InyGa1-y) obtained by the growth of the polycrystalline raw material LiXSe2 (X is equal to In / Ga / InyGa1-y) obtained by the invention can be controlled within 5 percent.

Description

technical field [0001] The invention belongs to a method for synthesizing polycrystalline compounds and single crystals, and relates to a method for synthesizing LiXSe 2 Methods for polycrystalline compounds and single crystals involving LiXSe for nonlinear optics and neutron detection 2 (X=In / Ga / In y Ga 1-y ) Preparation method of polycrystalline compound and single crystal. Background technique [0002] LiX 2 (X=In / Ga / In y Ga 1-y ) crystal is a nonlinear optical crystal with excellent performance. Based on its second-order nonlinear optical characteristics such as frequency multiplication, sum frequency, difference frequency, and optical parametric oscillation, it can be made into second harmonic generators, frequency converters, optical Nonlinear optical devices such as parametric oscillators. In addition, due to 6 Li has a large capture cross section for neutrons, and LiXSe 2 (X=In / Ga / In y Ga 1-y ) crystals can be prepared into neutron detectors, which are wid...

Claims

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Application Information

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IPC IPC(8): C30B29/52C30B11/02C30B28/06
CPCC30B29/52C30B11/02C30B28/06
Inventor 徐亚东郭力健薛望祺肖宝介万奇
Owner NORTHWESTERN POLYTECHNICAL UNIV
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