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Synthetic method for LiXSe2 polycrystalline compound and LiXSe2 single crystal

A synthesis method and compound technology, applied in selenium/tellurium compounds, chemical instruments and methods, metal selenide/telluride, etc., can solve problems such as insufficient reaction, insufficient melting of raw materials, insufficient contact, etc.

Pending Publication Date: 2019-12-03
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, all the raw materials are not melted enough, and the contact between Li, In, Ga and Se is not sufficient, especially the reaction between Se and Li is not sufficient enough to form Li 2 Se, In x Se y and Ga x Se y Compounds such as Li-Se, In-Se and Ga-Se formed cannot effectively fix Li and Se simple substances, and the loss of Se and Li cannot be obtained, so that the deviation of the stoichiometric ratio cannot be well reduced.

Method used

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  • Synthetic method for LiXSe2 polycrystalline compound and LiXSe2 single crystal
  • Synthetic method for LiXSe2 polycrystalline compound and LiXSe2 single crystal
  • Synthetic method for LiXSe2 polycrystalline compound and LiXSe2 single crystal

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Effect test

Embodiment 1

[0044] 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...

Embodiment 2

[0046] 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, Ga is completely melted, and Li and Se begin to react, which reduces Li's corrosion of the quartz crucible and the volatilization of Se at high temperatures. Then the temperature was raised to 220°C at a rate of 5°C / h...

Embodiment 3

[0048] 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, Ga is completely melted, and Li and Se start to react, reducing the corrosion of Li on the quartz crucible and the volatilization of Se at high temperatures. Then the tem...

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Abstract

The invention relates to a synthetic method for a LiXSe2 polycrystalline compound and a LiXSe2 single crystal. The method comprises the following steps: filling an crucible located at an inner layer and a quartz crucible with elementary substances such as Li, In, Ga and Se, performing vacuum packaging, packing quartz crucible into a swing furnace, performing heat preservation at the melting pointor higher of the LiXSe2 compound, performing shaking, and performing cooling to room temperature, wherein the obtained LiXSe2 (X=In / Ga / InyGa1-y) compound meets the stoichiometric ratio. According to the method provided by the invention, the temperature is controlled, the gradient-temperature heat preservation is adopted, at the lower vapor pressure of the Li and the Se, the four elementary substances including the Li, the In, the Ga and the Se are subjected to a combination reaction near the melting points of the Li and the Se to obtain compounds such as Li2Se, InxSey and GaxSey to immobilizethe chemical activity of the Li and the Se, so that the loss of the Li and Se components is reduced; and deviation of the chemical composition to the stoichiometric ratio of a LiXSe2 (X=In / Ga / InyGa1-y) single crystal obtained by growing the LiXSe2 (X=In / Ga / InyGa1-y) polycrystalline raw material obtained by using the method can be controlled within 5%.

Description

technical field [0001] The invention belongs to a method for synthesizing polycrystalline compounds and single crystals, and relates to a LiXSe 2 Synthesis methods of 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 widely used in nu...

Claims

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Application Information

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IPC IPC(8): C30B29/46C01B19/00C30B11/02
CPCC01B19/007C30B11/002C30B11/02C30B29/46
Inventor 徐亚东郭力健薛望祺肖宝介万奇
Owner NORTHWESTERN POLYTECHNICAL UNIV
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