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Hydrothermal preparation method capable of controlling thickness of tin selenide with sheet structure

A tin selenide, flake technology, applied in the direction of binary selenium/tellurium compound, metal selenide/telluride, nanotechnology, etc., can solve the problem of small thickness of flake pure phase SnSe, achieve small thickness and smooth operation process Simple, fast degradation effect

Active Publication Date: 2018-04-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many preparation methods of flaky SnSe, mainly including solvothermal method, precipitation method, hydrothermal method, etc., but there are few reports on the thickness control of flaky pure phase SnSe, especially in the process of preparing flaky SnSe by hydrothermal method. Among them, the thickness is about 150nm, but the applicant found that the thickness of flake SnSe is small, and its degradation rate to rhodamine B dye in the ultraviolet light region is just fast, so it is necessary to provide a method that can control the thickness of flake SnSe

Method used

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  • Hydrothermal preparation method capable of controlling thickness of tin selenide with sheet structure
  • Hydrothermal preparation method capable of controlling thickness of tin selenide with sheet structure
  • Hydrothermal preparation method capable of controlling thickness of tin selenide with sheet structure

Examples

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Effect test

Embodiment 1

[0027] 1) Weigh 1.2g of tartaric acid and dissolve it in 20mL of distilled water, stir until dissolved, then weigh 1mmol of tin dichloride and add it, stir until the solution is clear and transparent, and clear and transparent solution A is obtained. Weigh 1 mmol of selenium dioxide, 0.8 g of sodium hydroxide and 2 mmol of sodium borohydride into 15 mL of distilled water in sequence, and stir to obtain a transparent solution B.

[0028] 2) Slowly add the clear and transparent solution A to the transparent solution B, stir at room temperature for 10 min, then add 1 mmol 1,10-phenanthroline and stir evenly, then transfer to a polytetrafluoroethylene-lined autoclave, and then Put it in an oven for reaction, start from room temperature, raise the temperature to 180°C at a rate of 5°C / min, keep it warm for 12 hours, then cool the reaction system to room temperature naturally, turn on the hydrothermal kettle, collect samples by centrifugation, and dry under vacuum at 60°C After 5 ho...

Embodiment 2

[0033] 1) Weigh 1.2g of tartaric acid and dissolve it in 20mL of distilled water, stir until dissolved, then weigh 1mmol of tin dichloride and add it, stir until the solution is clear and transparent, and clear and transparent solution A is obtained. Weigh 1 mmol of selenium dioxide, 0.8 g of sodium hydroxide and 2 mmol of sodium borohydride into 15 mL of distilled water in sequence, and stir to obtain a transparent solution B.

[0034] 2) Slowly add the clear and transparent solution A to the transparent solution B, stir at room temperature for 10 minutes, then add 1 mmol of 2,2-bipyridine and stir evenly, then transfer to a polytetrafluoroethylene-lined autoclave, and then put React in an oven, start from room temperature, raise the temperature to 180°C at a rate of 5°C / min, keep it warm for 12 hours, then cool the reaction system to room temperature naturally, turn on the hydrothermal kettle, collect samples by centrifugation, and dry at 90°C for 1 hour in vacuum Afterwards...

Embodiment 3

[0037] 1) Weigh 1.2g of tartaric acid and dissolve it in 20mL of distilled water, stir until dissolved, then weigh 1mmol of tin dichloride and add it, stir until the solution is clear and transparent, and clear and transparent solution A is obtained. Weigh 1 mmol of selenium dioxide, 0.8 g of sodium hydroxide and 2 mmol of sodium borohydride into 15 mL of distilled water in sequence, and stir to obtain a transparent solution B.

[0038] 2) Slowly add the clear and transparent solution A to the transparent solution B, stir at room temperature for 10 minutes, then add 1 mmol of 4,4-bipyridine and stir evenly, then transfer to a polytetrafluoroethylene-lined autoclave, and then put React in an oven, start from room temperature, raise the temperature to 180°C at a rate of 5°C / min, keep it warm for 12 hours, then cool the reaction system to room temperature naturally, turn on the hydrothermal kettle, collect samples by centrifugation, and dry under vacuum at 70°C for 2 hours Afterw...

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Abstract

The invention provides a hydrothermal preparation method capable of controlling the thickness of tin selenide with a sheet structure. The hydrothermal preparation method comprises the following steps:dissolving tartaric acid in distilled water, then adding tin dichloride, and carrying out stirring until a solution is clear and transparent so as to obtain a solution A; then successively adding selenium dioxide, sodium hydroxide and sodium borohydride into distilled water so as to prepare a solution B; slowly adding the solution A into the solution B and carrying out stirring; then adding a morphological controlling agent 1,10-phenanthroline, 2,2-dipyridine or 4,4-dipyridyl, carrying out stirring, and then carrying out a reaction at 180 DEG C in a hydrothermal reaction vessel for 6-24 h; and successively carrying out centrifuging, washing and drying to obtain black tin selenide powder. According to the invention, the thickness of flaky SnSe is controlled by adding the morphological controlling agent in hydrothermal process; raw materials and the produced solutions in the whole process are easy to treat and have no pollution; and the hydrothermal preparation method is low in preparation cost, simple in operation process and high in repeatability, and can prepare high-purity flaky tin selenide.

Description

technical field [0001] The invention belongs to the technical field of hydrothermal synthesis of two-dimensional materials, and in particular relates to a hydrothermal preparation method for controlling the thickness of flake tin selenide. Background technique [0002] Tin selenide (SnSe) is a very important group IV-VI two-dimensional semiconductor material. Its constituent elements are abundant in the earth, non-toxic, and stable in chemical properties. SnSe layers are connected by weak van der Waals force, while electrons are confined in a two-dimensional environment, so they exhibit many unique physical and chemical characteristics. In photovoltaic (Li L, Chen Z, HuY, et al.Single-layer single-crystalline SnSe nanosheets[J].Journal of the American Chemical Society,2013,135(4):1213-6.), Thermoelectric (Zhao L D,Lo S H,Zhang Y,et al.Ultralow thermal conductivity and high thermoelectric figure of meritin SnSe crystals[J].Nature,2014,508(7496):373) and energy storage (Yuan ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y40/00
CPCC01B19/007C01P2002/72C01P2004/03C01P2004/20C01P2004/64
Inventor 张荔葛万银焦思怡叶晓慧李景雷常哲徐美美
Owner SHAANXI UNIV OF SCI & TECH
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