Preparation method of lead sulfide colloid quantum dots

A technology of colloidal quantum dots and lead sulfide, which is applied in the field of preparation of semiconductor nanomaterials, can solve the problems of complex synthesis process of quantum dots and poor repeatability of results, and achieve the effects of easy control, good reproducibility and easy storage.

Active Publication Date: 2020-09-08
NANCHANG UNIV
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Problems solved by technology

[0004] In order to solve the problem of complex synthesis process of quantum dots and poor repeatability of results, the present invention provides a preparation method of lead sulfide colloidal quantum dots. This patent uses a basic lead chloride material synthesized by a simple aqueous solution precipitation method as the lead source , to synthesize PbS quantum dots by reacting with elemental S

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  • Preparation method of lead sulfide colloid quantum dots

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Embodiment 1

[0020] A: Weigh 1.2g sodium chloride and 6g basic lead acetate (Pb(CH 3 COO) 2 ·Pb(OH) 2 ), and were dissolved in 15ml of distilled water respectively to prepare 1.37M and 0.7M solutions; then the two solutions were mixed and reacted at 80°C for 15min, and the white precipitate was rinsed with distilled water and dried to remove water to obtain basic lead chloride; Weigh 0.278g (0.001mol) of the synthesized basic lead chloride and 15ml of octylamine / oleic acid / octadecene mixed reagent, heat and react at 130°C for 30min under nitrogen protection, and then vacuumize for 30min to obtain the lead precursor solution;

[0021] B: Mix 0.032g (0.001mol) of elemental sulfur with 3.5ml of oleylamine at room temperature, and dissolve it quickly by ultrasonication to obtain a 0.286M sulfur precursor solution; then quickly inject the sulfur precursor solution into the step under a nitrogen atmosphere In the lead precursor solution described in A, cooled to 70°C; finally, cooled to 15°C ...

Embodiment 2

[0024] A: Weigh 1.2g sodium chloride and 6g basic lead acetate (Pb(CH 3 COO) 2 ·Pb(OH) 2 ), and were dissolved in 15ml of distilled water respectively to prepare 1.37M and 0.7M solutions; then the two solutions were mixed and reacted at 80°C for 15min, and the white precipitate was rinsed with distilled water and dried to remove water to obtain basic lead chloride; Weigh 0.278g (0.001mol) of the synthesized basic lead chloride and 15ml of oleylamine / oleic acid / octadecene mixed reagent, heat and react at 130°C for 30min under nitrogen protection, and then vacuumize for 30min to obtain the lead precursor solution;

[0025] B: Mix 0.032g (0.001mol) of elemental sulfur with 3.5ml of oleylamine at room temperature, and dissolve it quickly by ultrasonication to obtain a 0.286M sulfur precursor solution; then quickly inject the sulfur precursor solution into the step under a nitrogen atmosphere In the lead precursor solution described in A, cooled to 90°C; finally, cooled to 15°C ...

Embodiment 3

[0028] A: Weigh 1.2g sodium chloride and 6g basic lead acetate (Pb(CH 3 COO) 2 ·Pb(OH) 2 ), and were dissolved in 15ml of distilled water respectively to prepare 1.37M and 0.7M solutions; then the two solutions were mixed and reacted at 80°C for 15min, and the white precipitate was rinsed with distilled water and dried to remove water to obtain basic lead chloride; Weigh 0.278g (0.001mol) of the synthesized basic lead chloride and mix it with 15ml of octylamine / oleic acid / octadecene mixed reagent, heat and react at 130°C for 30min under the protection of nitrogen, then vacuumize for 30min to obtain the lead precursor body solution;

[0029] B: Mix 0.032g (0.001mol) of elemental sulfur with 3.5ml of oleylamine at room temperature, and dissolve it quickly by ultrasonication to obtain a 0.286M sulfur precursor solution; then quickly inject the sulfur precursor solution into the step under a nitrogen atmosphere In the lead precursor solution described in A, cooled to 120° C.; f...

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Abstract

The invention belongs to synthesis of semiconductor nanoparticles, and particularly relates to a preparation method of lead sulfide colloidal quantum dots. The preparation method disclosed by the invention comprises the following steps: heating submicron basic lead chloride as a lead source synthesized by an aqueous solution precipitation method and an organic reagent to form a lead precursor solution, then injecting the elemental sulfur solution dissolved in oleylamine into the lead precursor solution at a specific temperature to react for 0.5-20 minutes to obtain a lead sulfide colloidal quantum dot stock solution, and finally, carrying out impurity removal and anti-solvent purification to obtain the lead sulfide colloidal quantum dot solution. The preparation method disclosed by the invention has the advantages of good controllability, stable chemical properties of reactant raw materials, high fluorescence efficiency of reaction products and the like, and is suitable for batch synthesis of high-quality lead sulfide colloidal quantum dots.

Description

technical field [0001] The invention belongs to the field of preparation of semiconductor nanomaterials, and in particular relates to a preparation method of lead sulfide colloidal quantum dots. Background technique [0002] Quantum dots are a kind of semiconductor nanocrystals whose three-dimensional size is smaller than its Bohr radius, which has quantum confinement effect, and its emission / absorption range can be adjusted by controlling the size of nanocrystals. Among them, lead sulfide (PbS) quantum dots have the characteristics of continuously adjustable optical properties in the near-infrared wavelength range, and are widely used as key materials in many fields such as solar cells, photoluminescent diodes, biological imaging, and infrared image sensors. In the application process, the quality of quantum dots plays a crucial role in the performance of the corresponding device, which mainly depends on the synthesis process of quantum dots. [0003] At this stage, the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/66B82Y20/00B82Y40/00C01G21/21
CPCB82Y20/00B82Y40/00C01G21/21C09K11/661
Inventor 谭龙谭恋汤昊孙润光
Owner NANCHANG UNIV
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