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Method for preparing SnSe through solution method

A solution method and mixed solution technology, applied in the direction of metal selenide/telluride, binary selenium/telluride compound, etc., can solve the problems of adverse effects on the environment and operators, cumbersome preparation process, high cost, etc. The effect of being friendly to the operator, the preparation method is simple, and the handling is easy

Active Publication Date: 2019-03-29
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to prepare two-dimensional layered SnSe nanosheets, among several methods disclosed at present, including chemical vapor phase transport method, liquid phase method, and solid phase reaction method, these methods Some are expensive, some are cumbersome to prepare, and some involve the use of highly toxic reagents such as hydrazine hydrate in the synthesis process, resulting in adverse effects on the environment and operators during the preparation process

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  • Method for preparing SnSe through solution method
  • Method for preparing SnSe through solution method
  • Method for preparing SnSe through solution method

Examples

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Effect test

Embodiment 1

[0045] First, inject 20 mL of oleic acid into a 50 mL two-necked bottle, and disperse the selenium powder in the solvent to obtain the precursor solution A of the selenium source. Then put the two-neck bottle into the magnetic stirrer and add a thermometer, let the thermometer just touch the liquid surface, turn on the rotary button, observe whether the rotor will touch the thermometer, coat the thermometer and condenser tube with vaseline, and assemble the instrument. After the assembly of the instrument is completed, stir the mixed solution A, set the rotation speed at 550r / min, and the temperature at 100°C, turn on the vacuum pump to start vacuuming, and keep warm for 30min. Then, high-purity nitrogen gas was introduced to raise the temperature to 240°C and keep the temperature for 2h. Weigh 1mmol SnCl during 2 , Measure 30ml of absolute ethanol in a test tube, add SnCl 2 Dissolve in absolute ethanol to obtain three mixed solutions B. Cool the reaction down to 80°C, extr...

Embodiment 2

[0049] First, inject 20 mL of oleic acid into a 50 mL two-necked bottle, and disperse the selenium powder in the solvent to obtain the precursor solution A of the selenium source. Then put the two-neck bottle into the magnetic stirrer and add a thermometer, let the thermometer just touch the liquid surface, turn on the rotary button, observe whether the rotor will touch the thermometer, coat the thermometer and condenser tube with vaseline, and assemble the instrument. After the assembly of the instrument is completed, stir the mixed solution A, set the rotation speed to 500r / min, and the temperature to 130°C, turn on the vacuum pump to start vacuuming, and keep warm for 25min. Then pass high-purity argon to raise the temperature to 260°C and keep it warm for 1.5h. Weigh 1mmol SnCl during 2 , Measure 30ml of absolute ethanol in a test tube, add SnCl 2 Dissolve in absolute ethanol to obtain mixed solution B. Cool the reaction down to 85°C, extract 4ml of precursor solution A...

Embodiment 3

[0053] First, inject 20 mL of oleic acid into a 50 mL two-necked bottle, and disperse the selenium powder in the solvent to obtain the precursor solution A of the selenium source. Then put the two-neck bottle into the magnetic stirrer and add a thermometer, let the thermometer just touch the liquid surface, turn on the rotary button, observe whether the rotor will touch the thermometer, coat the thermometer and condenser tube with vaseline, and assemble the instrument. After the assembly of the instrument is completed, stir the mixed solution A, set the rotation speed at 600r / min, and the temperature at 110°C, turn on the vacuum pump to start vacuuming, and keep warm for 25min. Then, high-purity nitrogen gas was introduced to raise the temperature to 270°C and keep the temperature for 2h. Weigh 1mmol SnCl during 2 , Measure 30ml of absolute ethanol in a test tube, add SnCl 2 Dissolve in absolute ethanol to obtain mixed solution B. Cool the reaction down to 90°C, extract 3ml...

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Abstract

The invention discloses a method for preparing SnSe through a solution method. The method comprises the steps that selenium powder is dispersed into a high-boiling-point solvent to obtain a precursorsolution A of a selenium source; then, under the vacuum pumping condition, water vapor in the precursor solution A is removed, and the environment without oxygen and the water vapor is obtained; then,temperature increasing and heating treatment are conducted, the precursor solution A is extracted according to the proportion to be added into a mixed solution B composed of a tin source and ethyl alcohol, thus a mixed solution C is obtained, and then the mixed solution C is subjected to an alcohothermal reaction and then cooled to the room temperature; and through centrifugal separation, cleaning and drying, a black brown target product is obtained. According to the preparation method, the high temperature and high pressure are not needed, no highly toxic and hazardous substance is containedin reaction, inorganic tin salt serves as the tin source, the precursor solution is subjected to the alcohothermal reaction for several hours in a reaction kettle, thus the target product can be obtained, and the product is a purely-flaky nanosheet.

Description

technical field [0001] The invention belongs to the technical field of two-dimensional layered materials, and in particular relates to a method for preparing SnSe by a solution method. Background technique [0002] After graphene became a star material in the field of materials research, two-dimensional layered materials have received extensive attention. When the thickness of two-dimensional layered materials is reduced to the nanometer scale, or even atomic layer thickness, the two-dimensional layered materials show their strange physical, chemical, optical, electrical and other properties. First-class universities and research institutions at home and abroad have shown great interest in two-dimensional layered materials, and research has been carried out in full swing from the preparation methods of materials to their various functional applications. Among these materials, SnSe is an important P-type semiconductor material. Its constituent elements Sn and Se are abundant...

Claims

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Application Information

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IPC IPC(8): C01B19/04
CPCC01B19/007C01P2002/72C01P2004/03C01P2004/61
Inventor 张荔郭锐葛万银朱建峰
Owner SHAANXI UNIV OF SCI & TECH
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