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Method for preparing ternary alloy quantum dots in ole-morpholine solvent

A ternary alloy and oleoylmorpholine technology, which is applied to the preparation of CdSexS1-x (0) has high requirements for preparation conditions, unstable repeatability, and high cost of synthesis process, and achieves mild synthesis conditions, which are conducive to mass production and operation. easy effect

Active Publication Date: 2014-01-15
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In a word, the disadvantages of the existing ternary alloy quantum dot synthesis technology are: ①The synthesis process using phosphine as solvent and ligand is expensive, environmentally polluting, and has high requirements for preparation conditions; ②The existing thermal injection method operates The time is not easy to control, the repeatability is unstable, and it is not conducive to batch preparation

Method used

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  • Method for preparing ternary alloy quantum dots in ole-morpholine solvent
  • Method for preparing ternary alloy quantum dots in ole-morpholine solvent
  • Method for preparing ternary alloy quantum dots in ole-morpholine solvent

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Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: Preparation of CdSe 0.05 S 0.95 Ternary Alloy Quantum Dots

[0028] (1) Heat 0.130g (1mmol) cadmium oxide, 5mL (15mmol) oleic acid and 9mL oleoylmorpholine to dissolve, and then cool to room temperature to obtain a cadmium-containing precursor;

[0029] (2) Heat 0.004g (0.05mmol) Se powder, 0.030g (0.95mmol) S powder, and 3mL oleoylmorpholine to dissolve, and cool to room temperature to obtain a precursor solution containing Se and S;

[0030] (3) Add the above two precursor solutions into a 50mL three-necked bottle, heat it to 110°C under stirring, keep it warm for 1 hour to fully mix the two precursor solutions, and then heat it to 210°C at a heating rate of 15°C / min. °C, stop heating after 1 hour of reaction;

[0031] (4) Take out the reaction solution and add it to methanol at normal temperature to precipitate the crude product of quantum dots. After the crude product is centrifuged, washed, and dissolved in toluene, the CdSe-containing 0.05 S 0.9...

Embodiment 2

[0034] Embodiment 2: Preparation of CdSe 0.3 S 0.7 Ternary Alloy Quantum Dots

[0035] (1) Heat 0.266g (1mmol) cadmium acetate, 1.024g (4mmol) palmitic acid and 10mL oleoylmorpholine to dissolve, and then cool to room temperature to obtain a cadmium-containing precursor;

[0036] (2) Heat 0.024g (0.3mmol) Se powder, 0.022g (0.7mmol) S powder, and 4mL oleoylmorpholine to dissolve, and cool to room temperature to obtain a precursor solution containing Se and S;

[0037] (3) Add the above two precursor solutions into a 50mL three-neck bottle, heat it to 120°C under stirring, keep it warm for 50min to fully mix the two precursor solutions, and then heat it to 220°C at a heating rate of 12°C / min , stop heating after reacting for 2 hours;

[0038] (4) Take out the reaction solution and add it to methanol at normal temperature to precipitate the crude product of quantum dots. After centrifugation, washing, and dissolving with toluene, the CdSe-containing 0.3 S 0.7 Toluene soluti...

Embodiment 3

[0041] Embodiment 3: Preparation of CdSe 0.5 S 0.5 Ternary Alloy Quantum Dots

[0042] (1) Heat 0.678g (1mmol) cadmium stearate, 0.684g (3mmol) myristic acid and 10mL oleoylmorpholine to dissolve, then cool to room temperature to obtain a cadmium-containing precursor;

[0043] (2) Heat 0.039g (0.5mmol) Se powder, 0.016g (0.5mmol) S powder, and 5mL oleoylmorpholine to dissolve, and cool to room temperature to obtain a precursor solution containing Se and S;

[0044] (3) Add the above two precursors into a 50mL three-neck flask, and under the action of a magnetic stirring heating mantle, heat to 130°C, keep warm and stir for 40min to fully mix the two precursors, and then mix the two precursors at 10°C / The heating rate of min is heated to 230°C, and the heating is stopped after 3 hours;

[0045] (4) Take out the reaction solution and add it to propanol at room temperature, and precipitate the crude product of quantum dots. After centrifugation, washing, and dissolving with n...

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Abstract

The invention discloses a method for preparing CdSexS1-x ternary alloy quantum dots in ole-morpholine. The method is characterized in that: a precursor solution containing Cd and a precursor solution containing Se and S are respectively prepared with ole-morpholine as solvents; the two precursor solutions are mixed under a temperature of 110-130 DEG C; the mixture is heated to 220-250 DEG C with a heating speed of 10-15 DEG C / min, and is subject to a reaction for 1-3 hours; an obtained reaction liquid is injected into methanol, ethanol or propanol, such that a crude product is precipitated; the crude product is washed, processed through centrifugal separation, and is dissolved by using a non-polar organic solvent, such that CdSexS1-x is obtained, wherein 0<x<1. Therefore, a ternary alloy quantum dot solution is obtained. When the adopted molar ratio of Se / S is changed, quantum dots with different stoichiometric ratios can be prepared, wherein an emission spectrum is 450-646nm, and a half emission peak width is 32-48nm. The ternary alloy quantum dot synthesizing method provided by the invention is advantaged in simple operation and good repeatability. Also, the method is environment friendly, economic, and applicable.

Description

technical field [0001] The invention belongs to the technical field of ternary semiconductor nanomaterials, in particular to the preparation of CdSe in oleoylmorpholine solvent x S 1-x (0<x<1) method for ternary alloy quantum dots. Background technique [0002] According to the introduction in "Semiconductor Nanocrystal Quantum Dots" (Semiconductor Nanocrystal Quantum Dots, by Andrey L. Rogach, pages 1-72) published by Springer-Verlag / Wien in 2008, the size is smaller than that of the corresponding material Semiconductor nanocrystals with exciton Bohr radius are usually called quantum dots. Due to the quantum confinement effect, quantum dots have photoelectric properties related to size and shape. They can be applied to biological dyeing labels, photodiodes, single-electron lasers and quantum dots. Solar cells and other fields. At present, II-VI binary quantum dots, such as CdSe and CdS quantum dots, are the most researched. Quantum dots of different sizes are mainl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/88
Inventor 蒋阳王彬彬蓝新正李山鹰刘新梅
Owner HEFEI UNIV OF TECH
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