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Hydrothermal preparation method of bismuth selenide nano powder

A nano-powder, bismuth selenide technology, applied in nanotechnology, binary selenium/tellurium compounds, metal selenide/telluride and other directions, can solve the natural environment and human life hazards, the regulation and control limitations of powder morphology and size, etc. The problem is to achieve the effect of controllable morphology and size, low manufacturing cost, and simple and easy synthesis method.

Active Publication Date: 2020-02-04
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen from the above reports that although the hydrothermal method has been used to prepare bismuth selenide nanomaterials, because the synthesis reaction generally requires toxic reducing agents, metal organic salts or organic solvents, it will bring harm to the natural environment and human life. come to harm
In addition, the synthetically prepared Bi 2 Se 3 There are still limitations in terms of phase purity, crystallinity, and the adjustment and control of powder shape and size

Method used

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  • Hydrothermal preparation method of bismuth selenide nano powder
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  • Hydrothermal preparation method of bismuth selenide nano powder

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Dissolve 1.8g NaOH in 80ml pure water, stir to dissolve, add 0.006mol SeO 2 , continue stirring to become a colorless transparent solution, then add 0.004mol Bi(NO 3 ) 3 ·5H 2 O, continue to stir for 10 minutes, the solution turns into a beige mixed solution, and finally add 0.0075 mol of gallic acid (GA) to the above mixed solution, and continue to stir for 15 minutes to fully mix.

[0045] The above solution was transferred to a 100ml polytetrafluoroethylene reaction kettle, and the filling volume of the solution was 80%. It was placed in a preheated 200°C drying oven, reacted for 24 hours, and cooled naturally. Collect the black precipitate at the bottom of the hydrothermal reaction kettle and centrifuge at 4000rpm. The precipitate is washed three times with deionized water and once with absolute ethanol, and then dried in a vacuum oven at 60°C for 12 hours. , to obtain solid powder. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were performed on...

Embodiment 2

[0050] Dissolve 2.1g NaOH in 80ml pure water, stir to dissolve and add 0.006mol SeO 2 , stirred to become a colorless transparent solution, and then added 0.004mol Bi(NO 3 ) 3 ·5H 2 O, continue to stir for 10min, the solution turns into a beige mixed solution, add 0.01mol gallic acid (GA) to the above mixed solution, finally add 0.2g surfactant Triton X-100, stir until the solution is evenly mixed.

[0051] The above solution was transferred to a 100ml polytetrafluoroethylene reaction kettle, placed in a preheated 150°C drying oven, and reacted for 12h. After natural cooling, collect the black precipitate at the bottom of the hydrothermal reaction kettle, centrifuge the black precipitate at 5000rpm, then wash the precipitate with deionized water for 3 times, and then wash with absolute ethanol for 2 times. After drying in a vacuum oven for 12 hours, a solid powder was obtained. Carry out X-ray diffraction (XRD) and scanning electron microscope (SEM) detection to solid powd...

Embodiment 3

[0053] Dissolve 2.0g NaOH in 80ml pure water, stir and dissolve to form a colorless and transparent solution. Then add 0.006mol SeO 2 and 0.004mol BiCl 3 , stirred for 10 minutes, the solution turned into a beige mixed solution, added 0.01mol gallic acid (GA) to the above mixed solution, continued to stir for 15 minutes, then added 0.625g Triton X-100, and continued to stir until the solution was evenly mixed.

[0054] The above solution was transferred to a 100ml polytetrafluoroethylene reaction kettle, and heated in a dry oven preheated to 250°C for 24h. After cooling, collect the black precipitate at the bottom of the hydrothermal reaction kettle, centrifuge at 5000rpm to separate the solid, then wash with deionized water for 3 times and absolute ethanol for 2 times, and finally dry it in a vacuum oven at 60°C for 12 hours to obtain a solid powder product. X-ray diffraction (XRD) and scanning electron microscope (SEM) detection are carried out to it, and the XRD pattern ...

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Abstract

The invention relates to a hydrothermal preparation method of bismuth selenide nano powder. The hydrothermal preparation method specifically comprises the steps: S1, mixing and stirring raw materialsto obtain a reaction solution; and adding a surfactant according to the need of regulating and controlling the morphology of a powder crystal; S2, transferring the reaction solution obtained in the step S1 into a hydrothermal reaction kettle, carrying out a reaction at the temperature of 150 DEG C-250 DEG C for 12-36 h, and cooling to room temperature; and S3, carrying out centrifugal separation on the solution after the hydrothermal reaction to obtain solid powder, washing the solid powder with pure water and absolute ethyl alcohol for multiple times, and carrying out vacuum drying to obtainflaky or rod-like bismuth selenide nano-powder. The method is simple and easy to operate, toxic organic solvents and reducing agents are not used, the aqueous solutions and non-toxic raw materials areused, and the obtained product is pure in phase, high in crystallinity, controllable in size and morphology, high in product yield and environmentally friendly in preparation route.

Description

technical field [0001] The invention relates to a hydrothermal preparation method of bismuth selenide nano powder, which belongs to the field of nano material preparation. Background technique [0002] Bi 2 Se 3 The crystal belongs to the hexagonal crystal system, and its atomic arrangement is composed of five atomic layers connected by covalent bonds. The atomic layer arrangement is combined according to Se-Bi-Se-Bi-Se-, showing electrical neutrality. Bi 2 Se 3 It is a semiconductor material with a band gap of about 0.3eV. It has a very wide range of applications in thermoelectric conversion, refrigeration, biosensors, hydrogen storage materials, photovoltaic cell electrode materials and photocatalysis. In recent years, Bi 2 Se 3 It has also been found to be a new topological insulator material, which has the characteristics of surface conduction and internal insulation. This makes it have potential application value in the next generation of low-energy electronic de...

Claims

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Application Information

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IPC IPC(8): C01B19/04B82Y40/00
CPCC01B19/007B82Y40/00C01P2004/24C01P2004/16
Inventor 霍地吕梦凡
Owner NORTHEASTERN UNIV
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