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Preparation method of antimony sulfide nano rod

A technology of nanorods and antimony sulfide, applied in nanostructure manufacturing, chemical instruments and methods, nanotechnology, etc., can solve problems such as uneven size distribution, harsh preparation conditions, and poor product quality, and achieve excellent product quality and low implementation cost The effect of low and high thermal power

Inactive Publication Date: 2010-07-28
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses SbCl 3 Using thiourea as raw material, rod-shaped antimony sulfide nanomaterials with a length of 0.7-4 μm and a diameter of 40-360 nm and flower-shaped antimony sulfide nanomaterials with a size of 9-10 μm were prepared by reflux method, but the quality of the products obtained by this method is poor, and the size distribution of the rods is not good. Uniform: some rods are very short, but others are very long, and some of them are not rod-shaped granular substances, the preparation conditions are harsh and difficult to control

Method used

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  • Preparation method of antimony sulfide nano rod
  • Preparation method of antimony sulfide nano rod
  • Preparation method of antimony sulfide nano rod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Accurately weigh 1.6g Sb 2 o 3 Added to 50mL ethylene glycol (Sb 2 o 3 The ratio of the amount of substance with ethylene glycol is 1: 160), stir, and then add 1.0g of sulfur powder (the amount of substance of sulfur is Sb 2 o 3 5.6 times of the amount of substance), continue to stir and mix, and mixed solution is transferred in the three-necked flask.

[0023] (2) Slowly add 1.5 g of sodium borohydride (the amount of sodium borohydride substance is 1.26 times that of sulfur powder substance) into the mixed solution while stirring magnetically. Heated with an oil bath and refluxed at 185°C for 15 hours.

[0024] (3) Naturally cool to room temperature after the reaction, centrifuge, and remove the upper liquid to obtain a black precipitate. The obtained precipitates were alternately ultrasonically washed 3 times with deionized water and absolute ethanol respectively, and the obtained samples were dried in a constant temperature drying oven at 60°C for 8 hours t...

Embodiment 2

[0026] (1) Accurately weigh 1.6g Sb 2 o 3 Added to 60mL 1,2-propanediol (Sb 2 o 3 With 1, the ratio of the amount of substance of 2-propanediol is 1: 150), stir, then add 0.8g sulfur powder (the amount of substance of sulfur is Sb 2 o 3 4.5 times the amount of substance), continue to stir and mix, and the mixed solution is transferred to a three-necked flask.

[0027] (2) Slowly add 1.4 g of sodium borohydride (the amount of sodium borohydride substance is 1.48 times that of sulfur powder substance) into the mixed solution while magnetically stirring. Heated with an oil bath and refluxed at 175°C for 8 hours.

[0028] (3) Naturally cool to room temperature after the reaction, centrifuge, and remove the upper liquid to obtain a black precipitate. The obtained precipitates were alternately ultrasonically washed twice with deionized water and absolute ethanol respectively, and the obtained samples were dried in a constant temperature drying oven at 70°C for 6 hours to obtai...

Embodiment 3

[0030] (1) Accurately weigh 1.3g Sb 2 o 3 Added to 30mL 1,2-propanediol (Sb 2 o 3 With 1, the ratio of the amount of substance of 2-propanediol is 1: 92), stir, then add 1g sulfur powder (the amount of substance of sulfur is Sb 2 o 36.9 times of the amount of substance), continue to stir and mix, add surfactant polyethylene glycol 400 (PEG400) 3mL wherein (the amount of substance of polyethylene glycol 400 is Sb 2 o 3 1.9 times the amount of substance), after mixing, the mixed solution was transferred to a three-necked flask.

[0031] (2) Slowly add 1.3 g of sodium borohydride (the amount of sodium borohydride is 1.1 times the amount of sulfur powder) into the mixed solution while stirring magnetically. Heated with an oil bath and refluxed at 170°C for 8 hours.

[0032] (3) Naturally cool to room temperature after the reaction, centrifuge, and remove the upper liquid to obtain a black precipitate. The obtained precipitates were alternately ultrasonically washed 3 times...

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Abstract

The invention provides a preparation method of an antimony sulfide nano rod, which comprises the following steps: firstly, adding Sb2O3 into o-hydroxy diol and evenly stirring; secondly, adding sulphur powder and a surfactant for evenly stirring; thirdly, adding sodium borohydride and stirring and reflowing for a period of time, naturally cooling to room temperature and carrying out centrifuging separation to obtain black precipitation; and finally washing and drying the precipitation to obtain the antimony sulfide nano rod with the length of about 0.8-4.5mu m (micrometers), the diameter of 60-220nm (nanometers) and an orthorhombic phase and monocrystal structure. The method has the advantages of simple production equipment, safe production process, easily-controllable reaction parameters, high production efficiency, good dispersion performance of product particles for insusceptible aggregation, low implementation cost and easy industrial production. The invention can be widely applied to the preparation of a rod-shaped inorganic metal sulfur compound nanometer material.

Description

technical field [0001] The invention relates to a method for preparing inorganic functional nanometer materials, in particular to a method for preparing antimony sulfide nanorods by a reflux method. Background technique [0002] Antimony sulfide is a layered V-VI group direct bandgap semiconductor material with an energy bandgap of 1.5-2.2eV. It belongs to the orthorhombic crystal system and has high photosensitivity and high thermoelectric energy. It is widely used It is also an ideal material for utilizing solar energy in thermoelectric cooling technology, electronic and optoelectronic devices, and optoelectronics research in the infrared region. With the development of modern science and technology, it is recognized that the properties of nanomaterials depend on the shape and size of nanomaterials, such as nanoribbons, nanorods, nanofibers and nanotubes, etc. It has a wide range of uses due to its unique performance in mechanics and mechanics. Therefore, the preparation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/00B82B3/00
Inventor 朱启安雍高兵项尚陈利霞谭志刚徐军古
Owner XIANGTAN UNIV
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