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A method of a low -temperature two -phase synthesis method for cadmium sulfide quantum dots

A synthesis method, cadmium sulfide technology, applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of difficult to realize industrial production and increase the difficulty, and achieve the effects of narrow size distribution, uniform particle size, and low reaction temperature

Inactive Publication Date: 2015-09-23
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, from the perspective of the whole preparation process of the solvothermal method, the cadmium source and the sulfur source need to be mixed under high temperature conditions, and the nucleation and growth of nanocrystals need to be controlled at different high temperatures. The control of these conditions has increased the synthesis The difficulty makes this method difficult to achieve large-scale industrial production

Method used

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  • A method of a low -temperature two -phase synthesis method for cadmium sulfide quantum dots
  • A method of a low -temperature two -phase synthesis method for cadmium sulfide quantum dots
  • A method of a low -temperature two -phase synthesis method for cadmium sulfide quantum dots

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Experimental program
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Effect test

Embodiment 1

[0015] (1) Dissolve 0.025 mmol of cadmium nitrate in 1.25 ml of oleylamine, then add 5 ml of oleic acid to dilute to prepare a cadmium solution.

[0016] (2) Add 0.0056 g (0.175 mmol) of sublimed sulfur powder and 0.0324 g (0.0875 mmol) of trioctylphosphine to 5 ml of dimethyl sulfoxide, and ultrasonically dissolve the sublimed sulfur powder at room temperature to obtain sulfur solution.

[0017] (3) Mix the cadmium solution prepared in step (1) with the sulfur solution prepared in step (2), and react in a water bath at 70 degrees for 30 minutes. After the reaction, cadmium sulfide quantum dots are formed in the oil phase. Then extract the oil phase in the reaction system, add ethanol, centrifuge, wash the obtained yellow precipitate with toluene, add ethanol, centrifuge, and finally disperse with toluene as a solvent to obtain cadmium sulfide quantum dot sol.

[0018] The cadmium sulfide quantum dots prepared in this embodiment are characterized, and the transmission electro...

Embodiment 2

[0020] (1) Dissolve 0.025 mmol of cadmium sulfate in 1.25 ml of oleylamine, then add 5 ml of oleic acid to dilute to prepare a cadmium solution.

[0021] (2) Add 0.004 g (0.125 mmol) of sublimed sulfur powder and 0.0232 g (0.0625 mmol) of trioctylphosphine to 5 ml of dimethyl sulfoxide, and ultrasonically dissolve the sublimed sulfur powder at room temperature to obtain sulfur solution.

[0022] (3) Mix the cadmium solution prepared in step (1) with the sulfur solution prepared in step (2), and react in a water bath at 70 degrees for 30 minutes. After the reaction, cadmium sulfide quantum dots are formed in the oil phase. Then extract the oil phase in the reaction system, add ethanol, centrifuge, wash the obtained yellow precipitate with toluene, add ethanol, centrifuge, and finally disperse with toluene as a solvent to obtain cadmium sulfide quantum dot sol.

[0023] The cadmium sulfide quantum dots prepared in this embodiment are characterized, and the transmission electron...

Embodiment 3

[0025] (1) Dissolve 0.025 mmol of cadmium chloride in 1.25 ml of oleylamine, then add 5 ml of oleic acid to dilute to prepare a cadmium solution.

[0026] (2) Add 0.0016 g (0.05 mmol) of sublimed sulfur powder and 0.0093 g (0.025 mmol) of trioctylphosphine to 5 ml of dimethyl sulfoxide, and ultrasonically dissolve the sublimed sulfur powder at room temperature to obtain sulfur solution.

[0027] (3) Mix the cadmium solution prepared in step (1) with the sulfur solution prepared in step (2), and react in a water bath at 70 degrees for 30 minutes. After the reaction, cadmium sulfide quantum dots are formed in the oil phase. Then extract the oil phase in the reaction system, add ethanol, centrifuge, wash the obtained yellow precipitate with toluene, add ethanol, centrifuge, and finally disperse with toluene as a solvent to obtain cadmium sulfide quantum dot sol.

[0028] The cadmium sulfide quantum dots prepared in this embodiment are characterized, and the transmission electron...

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Abstract

The invention discloses a process for preparing cadmium sulfide quantum dots by a low temperature two-phase synthesis method. The process is as follows: a cadmium source is dissolved in oleylamine at room temperature, oleic acid is added for dilution to prepare a cadmium solution as an oil phase; the cadmium source is one of cadmium chloride, cadmium sulfate and cadmium nitrate, the volume ratio of oleylamine to oleic acid is 1:4; sublimated sulfur powder is ultrasonically dissolved in dimethyl sulfoxide containing tri-n-octylphosphine at room temperature to prepare a sulfur solution, or a sulfur compound is directly dissolved in the dimethyl sulfoxide containing the tri-n-octylphosphine to prepare a sulfur solution; the sublimated sulfur powder or the sulfur compound is used as a sulfur source, the sulfur compound is thiourea or sodium sulfide, the tri-n-octylphosphine is used as a wrapping agent, the molar ratio of sulfur source to wrapping agent is 2:1; the cadmium solution is mixed with the sulfur solution for reaction for 30 minutes under the condition of water bath at 70 DEG C, and the cadmium sulfide quantum dots are produced in the oil phase. The process has the advantages of wide raw material sources and low reaction temperature, the prepared cadmium sulfide quantum dots are uniform in particle size and narrow in size distribution, the absorption peak position can be adjusted between 396 to 445 nm, and the fluorescence is strong.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer material synthesis, in particular to a method for preparing cadmium sulfide quantum dots by a low-temperature two-phase synthesis method. Background technique [0002] Cadmium sulfide is an important II-VI direct bandgap semiconductor material with a bulk bandgap of 2.42eV and good absorption in the visible range. Cadmium sulfide whose size reaches the quantum dot level can absorb a photon to generate multiple electrons (multi-exciton effect) due to quantum effects, and its optical properties change with different sizes. These characteristics make cadmium sulfide quantum dots in catalysis, nonlinear optics , magnetic materials, optoelectronic devices, solar energy conversion, biology and communications and other fields have broader application prospects. Therefore, it is of great practical significance to synthesize cadmium sulfide quantum dot materials with controllable particle size...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/56
Inventor 利明邵飞燕杨建文
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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