Synthesis method of Sb2S3 nanorods

A synthesis method and nanorod technology, applied in the direction of nanotechnology, chemical instruments and methods, antimony compounds, etc., can solve problems such as complicated procedures, long reaction time, and lack of S, and achieve simple procedures, simple procedures, and good product quality Effect

CN110316756AInactive Publication Date: 2019-10-11HEBEI UNIVERSITY
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2019-10-11
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention provides a synthesis method of Sb2S3 nanorods. The method comprises the following steps that 1, high-purity sulfur and oleylamine are added into a reaction flask, vacuumizing is performed, and stirring and heating are performed at the same time; 2, when the temperature reaches 60 DEG C, nitrogen is replaced three times; 3, when the temperature reaches 90 DEG C, a nitrogen valve is turned on, and a vacuum pump is turned off; after sulfur is dissolved completely, the reaction is stopped; 4, SbCl3 is added into the reaction flask, then, octadecene and oleylamine are added, vacuumizing is performed, and stirring and heating are performed at the same time; 5, when the temperature reaches 60 DEG C, nitrogen is replaced three times; 6, when the temperature reaches 100 DEG C, the nitrogen valve is turned on, the vacuum pump is turned off, when the temperature is increased to 200 DEG C, a sulfur source is injected, after the reaction is performed for 5-20 min, heating is stopped,and the nanorods are obtained after centrifuging. According to the method for synthesizing antimony sulfide through a thermal injection method, the reaction time is greatly shortened, the crystallinestate can be achieved directly without annealing, and working procedures are simpler.
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Description

technical field

[0001] The invention relates to the technical field of nanomaterial preparation, in particular to a Sb 2 S 3 Synthesis of nanorods. Background technique

[0002] Antimony sulfide (Sb 2 S 3 ) is a binary direct bandgap compound that is an ideal photovoltaic material due to its bandgap covering the range of the solar spectrum. As an important group V-VI compound, antimony sulfide has attracted special attention because of its good photovoltaic properties, high thermoelectric power, spectral response, and suitable valence band position, with an energy band gap between 1.5 and 2.2 eV. , has been widely used in various fields such as solar cells and solid-state batteries, such as TV cameras with photoconductive targets, thermoelectric cooling devices, electronic and optoelectronic devices, etc. Studies on solar energy conversion and visible light-responsive photocatalysis have shown that the properties of antimony sulfide mainly depend on its crystal structur...

Examples

Embodiment 1

[0024] Such as figure 2 Shown, preparation process of the present invention is as follows:

[0025] (1) Preparation of sulfur source

[0026] Weigh 0.16g of high-purity sulfur (s, 99.99%) and place it in a three-necked flask, add 5mL of oleylamine (C 18 h 37 N, content 80-90%). Quickly connect the three-necked flask to the built device, turn on the vacuum pump to evacuate, turn on the heating mantle for heating and stirring (magnetic stirring), and when the reaction temperature reaches 60°C, open the nitrogen valve to fill the three-necked flask with nitrogen. Then evacuate again, and continue to heat up after replacing nitrogen three times like this. When the temperature reaches 90°C and the vacuum is pumped until there are no bubbles on the surface of the liquid, open the nitrogen valve and turn off the vacuum pump. Stop the reaction until all the sulfur in the three-necked flask is dissolved. When the temperature is cooled to 50°C, remove the three-necked flask, and ...

Embodiment 2

[0030] (1) Preparation of sulfur source

[0031] Weigh 0.16g of high-purity sulfur (s, 99.99%) into a three-necked flask, add 5mL of oleylamine (C 18 h 37 N, content 80-90%). Quickly connect the three-necked flask to the built device, turn on the vacuum pump to evacuate, turn on the heating mantle for heating and stirring (magnetic stirring), and when the reaction temperature reaches 60°C, open the nitrogen valve to fill the three-necked flask with nitrogen. Then evacuate again, and continue to heat up after replacing nitrogen three times like this. When the temperature reaches 90°C and the vacuum is pumped until there are no bubbles on the surface of the liquid, open the nitrogen valve and turn off the vacuum pump. Stop the reaction until all the sulfur in the three-necked flask is dissolved. When the temperature is cooled to 50°C, remove the three-necked flask, and put the prepared sulfur source into a vial for later use.

[0032] (2) Sb 2 S 3 preparation of

[0033]...

Embodiment 3

[0035] (1) Preparation of sulfur source

[0036] Weigh 0.16g of high-purity sulfur (s, 99.99%) into a three-necked flask, add 5mL of oleylamine (C 18 h 37 N, content 80-90%). Quickly connect the three-necked flask to the built device, turn on the vacuum pump to evacuate, turn on the heating mantle for heating and stirring (magnetic stirring), and when the reaction temperature reaches 60°C, open the nitrogen valve to fill the three-necked flask with nitrogen. Then evacuate again, and continue to heat up after replacing nitrogen three times like this. When the temperature reaches 90°C and the vacuum is pumped until there are no bubbles on the surface of the liquid, open the nitrogen valve and turn off the vacuum pump. Stop the reaction until all the sulfur in the three-necked flask is dissolved. When the temperature is cooled to 50°C, remove the three-necked flask, and put the prepared sulfur source into a vial for later use.

[0037] (2) Sb 2 S 3 preparation of

[0038]...