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Method for synthesizing tin selenide powder at room temperature

A room temperature synthesis, tin selenide technology, applied in the direction of metal selenide/telluride, binary selenium/telluride compounds, etc., can solve the problems of unhealthy operators, difficult to dissolve, environmental pollution, etc. Low heating and preparation costs

Active Publication Date: 2018-06-12
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 synthesis methods of tin selenide, mainly solvothermal method, hydrothermal method, etc. Some of these methods require special instruments in the preparation process, and some of them involve the use of toxic strong reduction agents such as hydrazine hydrate in the synthesis process. agent to reduce selenium source (SeO 2 )(Feng D, Ge Z H, Wu D, et al.Enhanced thermoelectric properties of SnSepolycrystals via texture control[J].Physical Chemistry Chemical Physics,2016,18(46):31821.), leading to environmental pollution during the preparation process and It is not good for the health of the operator; in addition, solvothermal method, hydrothermal method and other methods need to be heated at about 120°C-260°C, and surfactants need to be added, the process is complicated and time-consuming
The existing technology for synthesizing SnSe at room temperature uses Se powder as the source of selenium, but it is not easy to dissolve and needs to be dissolved with NaOH to release heat to about 80°C before it can be dissolved.

Method used

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  • Method for synthesizing tin selenide powder at room temperature
  • Method for synthesizing tin selenide powder at room temperature
  • Method for synthesizing tin selenide powder at room temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 2.4g of tartaric acid and dissolve it in 20mL of distilled water, stir until dissolved to obtain a clear and transparent solution, then add 2mmol of tin dichloride, stir until the solution becomes clear and transparent, and obtain solution A.

[0028] Add 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water in sequence, and stir evenly to obtain a transparent solution B.

[0029] Slowly add solution A to transparent solution B, stir at room temperature for 15 minutes, collect the sample by centrifugation, then put it in an oven for 3 hours at 60°C, and then cool it down to room temperature naturally to obtain black tin selenide powder.

[0030] figure 1 is the XRD spectrum of the product, no impurity peaks appear, indicating that the product is pure tin selenide.

[0031] figure 2 is the SEM photo of the product. From figure 2 It can be seen that the SnSe is agglomerated in granular form.

Embodiment 2

[0033] Weigh 2.34g of EDTA and dissolve it in 20mL of distilled water, stir until dissolved, then add 1mmol of tin dichloride to prepare solution A.

[0034] Add 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water in sequence, and stir evenly to obtain a transparent solution B.

[0035] Slowly add solution A to transparent solution B, stir at room temperature for 15 minutes, collect the sample by centrifugation, then put it in an oven for 3 hours at 65°C, and then cool it down to room temperature naturally to obtain black tin selenide powder.

[0036] image 3is the XRD spectrum of the product, no impurity peaks appear, indicating that the product is pure tin selenide.

[0037] Figure 4 is the SEM photo of the product. From Figure 4 It can be seen that lamellar SnSe is formed.

Embodiment 3

[0039] Weigh 2.31 g of citric acid and dissolve it in 20 mL of distilled water, stir until dissolved to obtain a clear and transparent solution, then add 2 mmol of tin dichloride, stir until the solution becomes clear and transparent, and obtain solution A.

[0040] Add 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water in sequence, and stir evenly to obtain a transparent solution B.

[0041] Slowly add solution A to transparent solution B, stir at room temperature for 15 minutes, collect the sample by centrifugation, then put it in an oven for 2 hours at 70°C, and then cool it down to room temperature naturally to obtain black tin selenide powder.

[0042] Figure 5 is the XRD spectrum of the product, no impurity peaks appear, indicating that the product is pure tin selenide.

[0043] Figure 6 is the SEM photo of the product. From Figure 6 It can be seen that SnSe is granular.

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Abstract

The invention discloses a precipitation method for synthesizing tin selenide powder at room temperature. The precipitation method comprises the following steps: dissolving tartaric acid, EDTA (Ethylene Diamine Tetraacetic Acid) or citric acid in distilled water; adding tin selenide and stirring till dissolution to obtain a solution A; adding selenium dioxide, sodium hydroxide and sodium borohydride into the distilled water in sequence to obtain a solution B; slowly adding the solution A into the solution B; stirring for 10 to 20 minutes; performing centrifugal separating, and collecting a sample; then, placing the sample into a drying oven for drying; then, naturally cooling to room temperature; drying to obtain black tin selenide powder. In the entire production process, raw materials andthe produced solutions are easy to treat and free from pollution; the method has the advantages of low preparation cost, simple operation process, short experiment time and high repeatability, and high-purity tin selenide powder can be prepared.

Description

technical field [0001] The invention relates to the technical field of room temperature synthesis of two-dimensional materials, in particular to a method for synthesizing tin selenide powder at room temperature. Background technique [0002] Tin selenide (SnSe) is a very important P-type semiconductor material with a two-dimensional layered structure, and the layers are connected by weak van der Waals force. The constituent elements of tin selenide are abundant in the earth and non-toxic, with stable chemical properties, narrow band gap (1.0-1.5eV), and excellent electronic and optoelectronic properties. SnSe has a wide range of potential applications, such as in photovoltaics (Li L, Chen Z, Hu Y, et al.Single-layer single-crystalline SnSenanosheets[J].Journal of the American Chemical Society,2013,135(4):1213 -6.), thermoelectric (Feng D, Ge Z H, Wu D, et al.Enhanced thermoelectric properties of SnSepolycrystals via texture control[J].Physical Chemistry Chemical Physics,201...

Claims

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Application Information

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