A preparation method for synthesizing three-dimensional stannous sulfide microflowers with quaternary ammonium salt auxiliary complexing agent

A technology of stannous sulfide and complexing agent, applied in chemical instruments and methods, inorganic chemistry, tin compounds, etc., can solve the problems of environmental pollution of waste liquid, many reaction steps, and complexity, and achieve simple preparation process, low cost, The effect of uniform size and shape

Inactive Publication Date: 2016-06-08
ZHANJIANG NORMAL UNIV
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  • Abstract
  • Description
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Problems solved by technology

Among them, in the method for preparing micro-nano materials with a three-dimensional hierarchical structure composed of stannous sulfide nanosheets, some need to use organic reagents such as polyols or ethylenediamine as solvents, and the waste liquid after the reaction is likely to pollute the environment; Others have many reaction steps and are complex
[0004] In this method, sodium sulfide is used as a complexing agent to convert positively charged tin ions into negatively charged thiostannate ions, and the quaternary ammonium salt tetrabutylammonium bromide is used as a morphology and structure regulator. The electrostatic interaction between positively charged tetrabutylammonium ions and negatively charged thiostannate ions uses hydrothermal and heat treatment techniques to synthesize a two-dimensional There is no public report on the method of stannous sulfide microflowers with three-dimensional hierarchical structure composed of nanosheets

Method used

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  • A preparation method for synthesizing three-dimensional stannous sulfide microflowers with quaternary ammonium salt auxiliary complexing agent
  • A preparation method for synthesizing three-dimensional stannous sulfide microflowers with quaternary ammonium salt auxiliary complexing agent
  • A preparation method for synthesizing three-dimensional stannous sulfide microflowers with quaternary ammonium salt auxiliary complexing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Dissolve 1mmol of tin tetrachloride in 10ml of deionized water to form solution A, dissolve 4mmol of sodium sulfide in 20ml of deionized water to form solution B; then add solution B dropwise to solution A to form a yellow precipitate, continue to drop Addition, the yellow precipitate gradually dissolved, and finally formed a transparent solution. Then 5mmol of tetrabutylammonium bromide (TBAB) and 4mmol of thiourea were added, and the final solution was transferred to a 50ml stainless steel reactor lined with polytetrafluoroethylene. Place it in a dry box, and conduct a hydrothermal reaction at 180° C. for 6 hours. Then it was naturally cooled to room temperature, and the obtained precipitate was rinsed three times with deionized water and absolute ethanol, separated by centrifugation, and dried in a vacuum oven at 60° C. for 12 hours. The hydrothermally obtained sample was placed in a tube furnace and calcined at 500° C. for 3 hours under the protection of nitrogen t...

Embodiment 2

[0032] Dissolve 1mmol of tin tetrachloride in 10ml of deionized water to form solution A, dissolve 4mmol of sodium sulfide in 20ml of deionized water to form solution B; then add solution B dropwise to solution A to form a yellow precipitate, continue to drop Addition, the yellow precipitate gradually dissolved, and finally formed a transparent solution. Then 3mmol of tetrabutylammonium bromide (TBAB) and 4mmol of thiourea were added, and the final solution was transferred to a 50ml stainless steel reactor lined with polytetrafluoroethylene. Put it in a dry box, and conduct a hydrothermal reaction at 170° C. for 4 hours. Then it was naturally cooled to room temperature, and the obtained precipitate was rinsed three times with deionized water and absolute ethanol, separated by centrifugation, and dried in a vacuum oven at 50° C. for 14 hours. The hydrothermally obtained sample was placed in a tube furnace and calcined at 400° C. for 2 hours under the protection of nitrogen to ...

Embodiment 3

[0034] Dissolve 0.5mmol of tin tetrachloride in 10ml of deionized water to form solution A, dissolve 2mmol of sodium sulfide in 20ml of deionized water to form solution B; then add solution B dropwise to solution A to form a yellow precipitate, continue Dropwise, the yellow precipitate gradually dissolved and finally formed a transparent solution. Then 2 mmol of tetrabutylammonium bromide (TBAB) and 2 mmol of thiourea were added, and the final solution was transferred to a 50 ml stainless steel reactor lined with polytetrafluoroethylene. Put it in a dry box, and conduct a hydrothermal reaction at 180° C. for 8 hours. Then it was naturally cooled to room temperature, and the obtained precipitate was rinsed three times with deionized water and absolute ethanol, separated by centrifugation, and dried in a vacuum oven at 70° C. for 10 hours. The hydrothermally obtained sample was placed in a tube furnace and calcined at 300° C. for 4 hours under the protection of nitrogen to obta...

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Abstract

The invention discloses a preparation method for synthesizing three-dimensional stannous sulfide micro-flowers with a quaternary ammonium salt auxiliary complexing agent, which belongs to the technical field of inorganic nanomaterial preparation; the step is to mix tin tetrachloride and complexing agent in a certain proportion under stirring Dissolve in deionized water to form a clear solution containing thiostannate complex ions, then add morphology and structure modifiers and sulfur sources under stirring, and transfer the reaction system to a stainless steel reactor lined with polytetrafluoroethylene placed in a drying oven, hydrothermally reacted at a certain temperature for a certain period of time, then naturally cooled to room temperature, rinsed the obtained precipitate with deionized water and absolute ethanol, centrifuged, and dried in a vacuum drying oven; after drying The sample is placed in a tube furnace, and calcined under nitrogen protection to obtain tin sulfide (SnS) micron flowers; the synthetic method of the present invention has the advantages of simple technique, low cost, and high yield, and the synthetic stannous sulfide The size and shape of micron flowers are relatively uniform, with an average diameter of 5 μm to 18 μm.

Description

technical field [0001] The invention relates to a preparation method of nanomaterials, in particular to a preparation method for synthesizing three-dimensional stannous sulfide microflowers with a quaternary ammonium salt auxiliary complexing agent, and belongs to the technical field of inorganic nanomaterial preparation. Background technique [0002] Inorganic micro-nano functional materials with controllable size and shape, especially micro-nano materials with three-dimensional hierarchical structure composed of nanostructures as basic units, have novel optical, electrical and electronic properties due to the advantages of both nanoscale and microscale. performance, which has aroused great interest and attention. Tin sulfide is an important semiconductor material with a direct bandgap of 1.2-1.5eV and an indirect bandgap of 1.0-1.1eV. It has high conversion efficiency and is a good material for preparing the absorbing layer of solar cell devices. In addition, the outstand...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/00
Inventor 马琳郭海燕徐旭耀周晓平
Owner ZHANJIANG NORMAL UNIV
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