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Method for preparing high-quality stannic sulfide nanosheet by use of single-source molecular precursor

A tin sulfide, high-quality technology, applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve the problems of many crystal defects, wide particle size distribution, and large product particle size, and achieve high crystallization degree and narrow particle size distribution , the effect of simple production equipment and process

Inactive Publication Date: 2012-05-30
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is the direct reaction method of elements; this method is generally carried out in a closed tube, which requires vacuum (or inert gas protection) and high reaction temperature (600-800 ° C), complicated operation, high energy consumption, and the synthesized product Large particle size, wide particle size distribution, many crystal defects, uneven composition and even a small amount of impurities

Method used

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  • Method for preparing high-quality stannic sulfide nanosheet by use of single-source molecular precursor
  • Method for preparing high-quality stannic sulfide nanosheet by use of single-source molecular precursor
  • Method for preparing high-quality stannic sulfide nanosheet by use of single-source molecular precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Weigh 5 mmol of crystalline tin tetrachloride, dissolve in absolute ethanol, and prepare a 100 mL solution; 2. Weigh 20 mmol of sodium diethyldithiocarbamate powder, add anhydrous ethanol to dissolve, and prepare a 100 mL solution; 3 . The tin tetrachloride solution prepared in step (1) is slowly added to the sodium diethyldithiocarbamate solution prepared in step (2) at normal temperature and under stirring, and kept stirring for 1 hour at normal temperature, then the resulting precipitation is Suction filtration, and put it in an oven to dry at 60°C for 12 hours to obtain the precursor Sn-(DDTC) 4 ;4. Take 1.0g precursor Sn-(DDTC) 4 Put it into a 50mL polytetrafluoroethylene-lined autoclave, add 40mL of 2.5% acetic acid aqueous solution as a solvent, seal the autoclave and place it in an electric oven, heat it at 180°C for 24 hours, and then stop heating , let it cool to room temperature naturally, filter the obtained precipitate with suction, wash with deionized ...

Embodiment 2

[0033] 1. Weigh 5 mmol of crystalline tin tetrachloride, dissolve in absolute ethanol, and prepare a 100 mL solution; 2. Weigh 20 mmol of sodium diethyldithiocarbamate powder, add anhydrous ethanol to dissolve, and prepare a 100 mL solution; 3 . The tin tetrachloride solution prepared in step (1) is slowly added to the sodium diethyldithiocarbamate solution prepared in step (2) at normal temperature and under stirring, and kept stirring for 1 hour at normal temperature, then the resulting precipitation is Suction filtration, and put it in an oven to dry at 60°C for 12 hours to obtain the precursor Sn-(DDTC) 4 ;4. Take 1.0g precursor Sn-(DDTC) 4 Put it into a 50mL polytetrafluoroethylene-lined autoclave, add 40mL of 5% acetic acid aqueous solution as a solvent, seal the autoclave, place it in an electric oven, heat it at 180°C for 24 hours, then stop heating and let It was naturally cooled to room temperature, the obtained precipitate was suction filtered, washed several times...

Embodiment 3

[0040] 1. Weigh 5mmol of crystalline tin tetrachloride, add absolute ethanol to dissolve, and make 100mL solution; 2. Weigh 20mmol sodium diethyldithiocarbamate powder, add absolute ethanol to dissolve, and make 100mL solution;

[0041] 3. The tin tetrachloride solution prepared in step (1) was slowly added to the sodium diethyldithiocarbamate solution prepared in step (2) at normal temperature and under stirring, and kept stirring for 1 hour at normal temperature, and then the obtained Precipitation and suction filtration, and put it in an oven to dry at 60 ° C for 12 hours to obtain the precursor Sn-(DDTC) 4 ;4. Take 1.0g precursor Sn-(DDTC) 4 Put it into a polytetrafluoroethylene-lined autoclave with a capacity of 50 mL, add 40 mL of 10% acetic acid aqueous solution as a solvent, seal the autoclave and place it in an electric oven, heat it at 180 ° C for 24 hours, then stop the heating, let It was naturally cooled to room temperature, the obtained precipitate was suction f...

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Abstract

The invention relates to a method for preparing a high-quality stannic sulfide nanosheet by use of single-source molecular precursor. The method comprises adding stannic chloride pentahydrate into anhydrous ethanol to prepare stannic chloride solution; dissolving sodium diethyldithiocarbamate powder in anhydrous ethanol to prepare sodium diethyldithiocarbamate solution; adding the stannic chloride solution into the sodium diethyldithiocarbamate solution, stirring, vacuum filtering and drying at 60 DEG C. to obtain a single-source molecular precursor Sn-(DDTC)4; putting the single-source molecular precursor Sn-(DDTC)4 into a high pressure vessel, and adding 2.5%-10% aqueous solution of acetic acid as solvent; and placing in an electric oven, heating at 180 DEG C. for 24 hours, cooling, vacuum filtering, washing by deionized water and anhydrous ethanol, and drying at 60 DEG C. to obtain yellow stannic sulfide powder. The invention overcomes the defects of an element direct reaction method and a chemical precipitation method, involves a low-toxicity easily-accessible single-source molecular precursor with reasonable price, simplifies the preparation process, and easily obtains a uniform-composition pure phase nanomaterial conforming to stoichiometric ratio. The obtained product has high crystallization degree and is nanosheet-like pure hexagonal phase stannic sulfide.

Description

technical field [0001] The invention relates to a high-quality tin sulfide nanosheet of a semiconductor material, belonging to the field of novel optoelectronic functional materials, in particular to a method for preparing high-quality tin sulfide nanosheets by using a single source molecular precursor. Background technique [0002] Tin Sulfide (SnS 2 ) is an n-type semiconductor (with a band gap of 2.2 eV at room temperature) with excellent optical, electrical, gas-sensing and photocatalytic properties, which can be used as semiconductor materials, photoconductive and photosensitive materials, and window absorbing materials in solar cells , Lithium battery anode materials, gas sensor materials and photocatalytic materials, etc. In addition, SnS 2 It has a brilliant golden yellow, also known as pseudo-gold or gold-like powder. It is a high-grade colorant, which can replace the widely used gold powder paint (copper powder) for urban construction, advertising, printing, deco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/00B82Y40/00
Inventor 张永才杜珍妮张明
Owner YANGZHOU UNIV
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