Preparation method of silver sulfide quantum dots

A technology of quantum dots and silver sulfide, which is applied in the field of semiconductor nanomaterial preparation, can solve problems such as difficult storage, low particle fluorescence quantum efficiency, and complicated experimental operations, and achieve good near-infrared luminescence properties, good fluorescence quantum efficiency, and simple reaction operations Effect

Inactive Publication Date: 2013-01-02
JILIN UNIV
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Problems solved by technology

With the development of synthesis technology, in 2010, the Wang group reported the preparation of Ag with a size above 5nm by thermal decomposition of unit organic precursors. 2 S quantum dots (J.Am.Chem.Soc.2010,132,1470), and the Ag synthesized by this method 2 S quantum dots have near-infrared optical properties, but this method requires a high temperature above 200 ° C, the particle fluorescence quantum efficiency of the prepared particles is relatively low, and the absorption spectrum is not obvious
Not long ago, the Pang group synthesized Ag with a smaller size (about 1.5~2.8nm) 2 S quantum dots (Chem.Mater.2012, 24, 3) have very obvious near-infrared absorption, and the fluorescence quantum efficiency reaches 0.18%. The TMS-S used in it ...

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  • Preparation method of silver sulfide quantum dots
  • Preparation method of silver sulfide quantum dots
  • Preparation method of silver sulfide quantum dots

Examples

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Embodiment 1

[0028] First, prepare sulfur-octadecene (S-ODE for short) infusion solution. Take 10 mmol of sulfur elemental substance and place it in 20 mL of octadecene (abbreviated as ODE), and dissolve it by ultrasonic waves to prepare a 0.5 mol / L S-ODE injection solution, which is a light yellow transparent solution. 0.4mmol of silver acetate powder, 0.8mmol of oleic acid, and 10mL of LODE were placed in a three-necked flask, injected with 2mmol of 6-alkylmercaptool, heated to 60°C, vacuumed three times with nitrogen, heated to 120°C, and quickly injected 0.4 mL of the S-ODE solution with a concentration of 0.5 mol / L configured above, and keep the temperature for 20 minutes to obtain Ag 2 S quantum dots, its absorption, emission and excitation spectra are shown in figure 1 As shown, the transmission electron microscope pictures are shown as figure 2 As shown, the X-ray diffraction pattern is shown in image 3 As shown, the prepared Ag 2 The size of S quantum dots is about 2.5nm...

Embodiment 2

[0035] Take 0.4mmol of silver acetate powder, 0.8mmol of oleic acid, and 10mL of solvent ODE in a three-necked flask, inject 2mmol of 12-alkylmercaptool, raise the temperature to 60°C through an electric heating mantle, vacuumize for 30 minutes, and then pass through the protection Gas nitrogen, repeat twice, then raise the temperature to 120°C, quickly inject 0.4mL of the prepared S-ODE solution with a concentration of 0.5mol / L described in Example 1, and keep the temperature for 20 minutes to obtain Ag 2 S quantum dots are only relatively uneven in size distribution, and the corresponding absorption spectrum peaks are not sharp and symmetrical. The fluorescence quantum efficiency measured by the measurement method described in Example 1 is 0.76%.

Embodiment 3

[0037] Take 0.4mmol of silver acetate powder, 0.8mmol of oleic acid, and 10mL of LODE in a three-necked flask, inject 2mmol of 18-alkylmercaptol, heat up to 60°C, vacuum three times with nitrogen, heat up to 120°C, and quickly inject 0.4 mL of the prepared S-ODE solution with a concentration of 0.5 mol / L described in Example 1, keep the temperature and react for 10 minutes to obtain Ag 2 The S quantum dots are only relatively inhomogeneous in size distribution, and the absorption spectrum has no obvious peaks, and has fluorescent properties. The fluorescent quantum efficiency measured by the measurement method described in Example 1 is 0.4%.

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Abstract

The invention provides a preparation method of silver sulfide quantum dots, belonging to the technical field of the preparation of semiconductor nanometer materials. The invention mainly provides a novel method for preparing the Ag2S quantum dots with the near infrared fluorescent property, comprising the following steps of: obtaining the quantum dots by a method of thermal injection in non-coordination agent under a relative low temperature due to an organic ligand which is provided with sulfydryl of a short chain, and precipitating in acetone or ethanol and dispersing into chloroform or hexane solvent. The quantum dots prepared by the invention have the fluorescent property at a near infrared region, has certain quantum efficiency and good monodispersity and stability, is uniform in particle size, and the size of the particle does not need selecting, so that the preparation method is simple to operate and low in cost.

Description

technical field [0001] The invention belongs to the technical field of semiconductor nano material preparation. It relates to a new method for preparing semiconductor quantum dots with good monodispersity and near-infrared fluorescence properties. Background technique [0002] After the semiconductor material gradually decreases from the bulk phase to a certain critical size (1-20 nanometers), the volatility of its carriers becomes significant, and the movement will be limited, resulting in an increase in kinetic energy. The corresponding electronic structure is continuous from the bulk phase to The energy level structure becomes a quasi-split discontinuity, a phenomenon known as the quantum size effect. The more common semiconductor nanoparticles, that is, quantum dots, mainly include II-VI, III-V and IV-VI groups. These types of quantum dots are well obeyed by the quantum size effect, and their properties change regularly with the size, for example, the absorption and em...

Claims

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Application Information

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IPC IPC(8): C01G5/00B82Y30/00
Inventor 解仁国李冬泽杨文胜
Owner JILIN UNIV
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