Preparation method of monodisperse PbS quantum dot

A technology of lead sulfide and quantum dots, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as difficulties in large-scale production, high cost of sulfur sources, and easy volatility, and achieve low cost of equipment and raw materials, low cost, and easy operation. The effect of simple process

Active Publication Date: 2017-02-22
深圳市联宝威科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the sulfur source (bis-trimethylsilylsulfide) widely used in the quantum synthesis of lead sulfide is relatively expensive, highly volatile and has certain toxicity, which makes it difficult for large-scale production

Method used

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  • Preparation method of monodisperse PbS quantum dot
  • Preparation method of monodisperse PbS quantum dot
  • Preparation method of monodisperse PbS quantum dot

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method of monodisperse lead sulfide quantum dots, comprising the steps of:

[0026] S1. Mix 0.834g (0.003mol) of lead chloride with 10mL of oleylamine, heat to 100°C and stir for 30 minutes to obtain a lead precursor. The concentration of lead in the lead precursor is about 0.3mol / L, and then cool down to 20°C ,spare;

[0027] S2. Stir 0.075g (0.001mol) thioacetamide and 2mL oleylamine at 20°C for 20min to form a sulfur precursor, the concentration of sulfur in the sulfur precursor is about 0.5mol / L;

[0028] S3. At a temperature of 20°C, mix the lead precursor in S1 and the sulfur precursor in S2 and stir rapidly (wherein the molar ratio of lead to sulfur is 3:1), the stirring speed can be selected according to experience, for example, it can be selected as 100-500r / min, then heated to 70°C and kept for 15min;

[0029] S4. Cool the solution after the heat preservation in S3 to 20° C., inject 8 mL of oleic acid to remove the residual lead precursor;

[...

Embodiment 2

[0037] A preparation method of monodisperse lead sulfide quantum dots, comprising the steps of:

[0038] S1. Mix 1.391g (0.005mol) of lead chloride with 10mL of oleylamine, heat to 140°C and stir for 40min to obtain a lead precursor, the concentration of lead in the lead precursor is about 0.5mol / L, and then cool down to 28°C ,spare;

[0039] S2. Stir 0.075g (0.001mol) thioacetamide and 20mL oleylamine at 28°C for 20min to form a sulfur precursor, the concentration of sulfur in the sulfur precursor is about 0.05mol / L;

[0040] S3. At a temperature of 28°C, mix the lead precursor in S1 and the sulfur precursor in S2 and stir rapidly (the molar ratio of lead to sulfur is 5:1), then heat to 90°C and keep it warm for 120min;

[0041] S4. Cool the solution after the heat preservation in S3 to 28° C., and inject 25 mL of oleic acid to remove the residual lead precursor;

[0042] S5. Add n-hexane and ethanol and centrifuge to obtain lead sulfide quantum dots coated with oleic acid ...

Embodiment 3

[0045] A preparation method of monodisperse lead sulfide quantum dots, comprising the steps of:

[0046] S1. Mix 0.734g (0.002mol) of lead bromide with 10mL of oleylamine, heat to 190°C and stir for 20min to obtain a lead precursor, the concentration of lead in the lead precursor is about 0.2mol / L, and then cool down to 35°C ,spare;

[0047] S2. Stir 0.075g (0.001mol) thioacetamide and 1mL oleylamine at a temperature of 35°C for 20min to form a sulfur precursor, the concentration of sulfur in the sulfur precursor is about 1mol / L;

[0048] S3. At a temperature of 20°C, mix the lead precursor in S1 and the sulfur precursor in S2 and stir rapidly (the molar ratio of lead to sulfur is 2:1), then heat to 60°C and keep it warm for 25min;

[0049]S4. Cool the solution after the heat preservation in S3 to 35° C., inject 4 mL of oleic acid to remove the residual lead precursor;

[0050] S5. Add n-hexane and ethanol and centrifuge to obtain lead sulfide quantum dots coated with oleic ...

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Abstract

The invention belongs to the technical field of preparation of compound semiconductor nanomaterials and particularly relates to a preparation method of a monodisperse PbS quantum dot. The method comprises steps as follows: S1, a halide of lead and oleylamine are mixed, heated to 80-190 DEG C and fully stirred to form a lead precursor, and then the lead precursor is cooled to 20-35 DEG C; S2, thioacetamide and oleylamine are fully stirred at 20-35 DEG C to form a sulfur precursor; S3, the lead precursor and the sulfur precursor are mixed in the molar ratio of Pb and S being (2-5):1, heated to 60-90 DEG C and subjected to heat preservation for a certain period; S4, the solution after heat preservation in S3 is cooled to 20-35 DEG C, and oleic acid is added to remove the residual lead precursor; S5, the PbS quantum dot is obtained after separation and purification. The prepared PbS quantum dot has the characteristics of high crystallinity, size uniformity, oleic acid and halogen mixed passivation, efficient luminescence, high stability and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of compound semiconductor nanomaterials, and in particular relates to a preparation method of monodisperse lead sulfide quantum dots. Background technique [0002] Quantum dots (semiconductor nanocrystals) are semiconductor nanoparticles synthesized by solution process. Due to the quantum size effect, their bandgap can be precisely adjusted by size, and then their optical properties can be adjusted. Therefore, quantum dots have become an important class of optical and optoelectronic materials. Lead sulfide is a narrow bandgap semiconductor, so the optical properties of lead sulfide quantum dots can be tuned in the entire near-infrared range, thus becoming a new material for solar cells and photodetectors. For example, a company (Lianghong Technology) has used lead sulfide quantum dots to make image sensors to replace the widely used CCD cameras on mobile phones. The efficiency of solar cells...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/66C09K11/02
CPCC09K11/025C09K11/661
Inventor 张建兵马铭张海波简卫
Owner 深圳市联宝威科技有限公司
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