Preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through complexing agent with aid of quaternary ammonium salt

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

Inactive Publication Date: 2014-02-19
ZHANJIANG NORMAL UNIV
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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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  • Preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through complexing agent with aid of quaternary ammonium salt
  • Preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through complexing agent with aid of quaternary ammonium salt
  • Preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through complexing agent with aid of quaternary ammonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0031] 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

[0033] 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 samples were placed in a tube furnace and calcined at 400°C for 2 hours under the protection of nitrogen to ...

Embodiment 3

[0035] 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 then 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...

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Abstract

The invention discloses a preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through a complexing agent with the aid of quaternary ammonium salt and belongs to the technical field of preparation of inorganic nano-materials. The method comprises the following steps: dissolving stannic chloride and the complexing agent into deionized water at a certain ratio while stirring to form a settled solution containing thiostannate radical complexing ions, then adding a shape and structure modifier and a sulfur source during stirring, and transferring the reaction system into a stainless-steel reaction kettle lined with polytetrafluoroethylene; placing the reaction kettle in a drying oven, performing hydrothermal reaction for a certain time at a certain temperature, then performing natural cooling to room temperature, rinsing obtained sediments with deionized water and absolute ethyl alcohol respectively, performing centrifugal separation, and performing drying in a vacuum drying oven; placing dried samples in a tube furnace, calcining the samples under nitrogen protection to obtain the stannous sulfide (SnS) micro-flowers. The synthetic method provided by the invention has the advantages of simple process, low cost and high yield; the synthetized stannous sulfide micro-flowers are relatively uniform in size and shape and have the average diameter of 5-18Mum.

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 Applications(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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