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Method for preparing quantum dots by taking sublimed sulfur as sulfur source

A technology for sublimating sulfur and quantum dots, which is applied in the preparation/purification of sulfur, chemical instruments and methods, sulfur compounds, etc., can solve the problems of low quantum yield, long reaction time, and low quantum yield of sulfur quantum dots, and achieve Good dispersion, enhanced fluorescence intensity, and wide application prospects

Inactive Publication Date: 2021-02-02
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the low quantum yield of sulfur quantum dots, complicated preparation, long reaction time and other limitations make it still have a lot of room for improvement.
[0005] In view of the low quantum yield, cumbersome preparation and long reaction time of the current preparation methods of sulfur quantum dots, it is of great application value to explore efficient methods and select high-quality elemental sulfur resources to synthesize sulfur quantum dots

Method used

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  • Method for preparing quantum dots by taking sublimed sulfur as sulfur source
  • Method for preparing quantum dots by taking sublimed sulfur as sulfur source
  • Method for preparing quantum dots by taking sublimed sulfur as sulfur source

Examples

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Embodiment 1

[0018] This embodiment provides a method for preparing quantum dots using sublimated sulfur as a sulfur source, and the specific preparation method is as follows.

[0019] (1) Add 2 g of sodium hydroxide, 3 mL of polyethylene glycol (PEG-400) and 2 g of sublimed sulfur to 50 mL of deionized water, and react in a water bath at 40 °C for 45 h to obtain a mixed solution.

[0020] (2) Change the mixed solution obtained in step (1) from water bath reaction to ice bath reaction. Under stirring conditions, 10 mL of hydrogen peroxide by weight was added to prepare a sulfur quantum dot solution with blue fluorescence characteristics.

[0021] (3) Add anti-solvent acetone to settle the water-soluble sulfur quantum dots, and then centrifuge the sulfur quantum dots precipitated from the aqueous solution at a speed of 9000 r / min for 5 minutes, and freeze-dry the obtained precipitate (drying temperature - 30 °C, 12 hours), and finally white sulfur quantum dot powder was obtained.

Embodiment 2

[0023] This embodiment provides a method for preparing quantum dots using sublimated sulfur as a sulfur source, and the specific preparation method is as follows.

[0024] (1) Add 3.5 g of sodium hydroxide, 3 mL of polyethylene glycol (PEG-400) and 4 g of sublimed sulfur to 50 mL of deionized water, and react in a water bath at 60 °C for 20 h to obtain a mixed solution.

[0025] (2) Change the mixed solution obtained in step (1) from water bath reaction to ice bath reaction. Under stirring conditions, 10 mL of hydrogen peroxide by weight was added to prepare a sulfur quantum dot solution with blue fluorescence characteristics.

[0026] (3) Add anti-solvent acetone to settle the water-soluble sulfur quantum dots, and then centrifuge the sulfur quantum dots precipitated from the aqueous solution at a speed of 9000 r / min for 5 minutes, and freeze-dry the obtained precipitate (drying temperature - 30 °C, 12 hours), and finally white sulfur quantum dot powder was obtained.

Embodiment 3

[0028] This embodiment provides a method for preparing quantum dots using sublimated sulfur as a sulfur source, and the specific preparation method is as follows.

[0029] (1) Add 5 g of sodium hydroxide, 3 mL of polyethylene glycol (PEG-400) and 7 g of sublimed sulfur to 50 mL of deionized water, and react in a water bath at 70 °C for 10 h to obtain a mixed solution.

[0030] (2) Change the mixed solution obtained in step (1) from water bath reaction to ice bath reaction. Under stirring conditions, 20 mL of hydrogen peroxide by weight was added to prepare a sulfur quantum dot solution with blue fluorescent properties.

[0031] (3) Add anti-solvent acetone to settle the water-soluble sulfur quantum dots, and then centrifuge the sulfur quantum dots precipitated from the aqueous solution at a speed of 9000 r / min for 5 minutes, and freeze-dry the obtained precipitate (drying temperature - 30 °C, 15 hours), and finally white sulfur quantum dot powder was obtained.

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Abstract

The invention provides a method for preparing quantum dots by using sublimed sulfur as a sulfur source, and belongs to the field of nano material preparation. The preparation method is characterized by comprising the following steps: (1) respectively adding 0.5-6 g of sodium hydroxide, 3mL of polyethylene glycol (PEG400) and 1-10g of sublimed sulfur into 50mL of deionized water, and carrying out water bath reaction at 40-80 DEG C for 3-50 hours to obtain a mixed solution; (2) changing the mixed solution obtained in the step (1) from a water bath reaction to an ice bath reaction, and under a stirring condition, adding 10-50 mL of hydrogen peroxide in parts by weight to prepare a sulfur quantum dot solution with blue fluorescence characteristics; and (3) adding an anti-solvent acetone to settle the water-soluble sulfur quantum dots, centrifuging the sulfur quantum dots settled from the aqueous solution at a centrifugal rotating speed of 9000 r / min for 5 min, and freeze-drying the obtained precipitate (at a drying temperature of -30 DEG C for 12-18 h) to finally obtain white sulfur quantum dot powder. The preparation process is green, safe and easy to prepare, fluorescence intensity is enhanced, dispersity is good, and efficiency is high.

Description

technical field [0001] The invention provides a method for preparing quantum dots by using sublimed sulfur as a sulfur source, and belongs to the field of nanometer material preparation. Background technique [0002] Energy, new materials, biotechnology and information technology together constitute the four pillars of a civilized society. Among them, materials are the material basis of information and energy. Since the beginning of the 21st century, human beings have gradually deepened their research on materials, among which nanomaterials have attracted widespread attention due to their special physical and chemical properties. [0003] Among nanomaterials, quantum dots have attracted much attention due to their special optical properties. Quantum dots are zero-dimensional nanomaterials with quantum effects, and their size is strictly limited. This limitation makes the size of the material smaller than the free path of electrons, resulting in local interaction, so its e...

Claims

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Application Information

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IPC IPC(8): C09K11/56B82Y20/00B82Y40/00C01B17/02
CPCC09K11/56B82Y20/00B82Y40/00C01B17/0243
Inventor 王依山张学谦温广武
Owner SHANDONG UNIV OF TECH
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