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A kind of preparation method of ultra-small silver sulfide quantum dots

A technology of silver sulfide and quantum dots, applied in the field of nanomaterials, can solve the problems of small size preparation and size regulation difficulty, poor dispersion of silver sulfide quantum dots, etc., and achieve the effects of high reproducibility, good crystallinity and uniform size distribution

Active Publication Date: 2022-03-25
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above-mentioned technical status, the purpose of the present invention is to provide a method for preparing ultra-small silver sulfide quantum dots, which aims to solve the problems of poor dispersion, small size preparation and size control of silver sulfide quantum dots

Method used

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  • A kind of preparation method of ultra-small silver sulfide quantum dots
  • A kind of preparation method of ultra-small silver sulfide quantum dots
  • A kind of preparation method of ultra-small silver sulfide quantum dots

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Embodiment 1

[0022] First, 0.6 g single-source precursor silver N,N-diethyldithiocarbamate (AgS 2 CN(C 2 h 5 ) 2 ) powder was ultrasonically dispersed into 90 g of N,N-dimethylformamide / N-methylpyrrolidone mixed solvent (1:1 volume ratio), and then poured into a polytetrafluoroethylene reactor; at 240°C After cooling for 120 min, the reaction solution was centrifuged at 6000 rpm for 10 min to separate the product. The product was washed with a mixed solvent of N,N-dimethylformamide and N-methylpyrrolidone several times and then washed with absolute ethanol. The washed product was finally dried at 60°C for 2 hours to obtain silver sulfide quantum dots. Perform XRD analysis on the dried powder sample, and re-disperse it ultrasonically into the above mixed solvent for TEM test.

[0023] XRD and TEM of silver sulfide quantum dots such as figure 1 , figure 2 shown. figure 1 It shows that the material synthesized by thermal decomposition of single-source precursor is silver sulfide cryst...

Embodiment 2

[0025] First, 0.7 g single-source precursor silver N,N-dibutyldithiocarbamate (AgS 2 CN(C 4 h 9 ) 2 ) powder was ultrasonically dispersed into 90 g of N,N-dimethylformamide / N-methylpyrrolidone mixed solvent (1:1 volume ratio), and then poured into a polytetrafluoroethylene reactor; at 240°C After cooling for 120 min, the reaction solution was centrifuged at 6000 rpm for 10 min to separate the product. The product was washed with a mixed solvent of N,N-dimethylformamide and N-methylpyrrolidone several times and then washed with absolute ethanol. The washed product was finally dried at 60°C for 2 hours to obtain silver sulfide quantum dots. The dried powder sample was re-dispersed ultrasonically into the above mixed solvent for TEM testing.

[0026] TEM of silver sulfide quantum dots as image 3 shown. image 3 It shows that the size of the synthesized silver sulfide quantum dots is very small, ranging from 1.4 to 2.3 nm, and the dispersion is very uniform.

Embodiment 3

[0028] First, 0.9 g single-source precursor silver N,N-di-n-hexyldithiocarbamate (AgS 2 CN(C 6 h 13 ) 2 ) powder was ultrasonically dispersed into 90 g of N,N-dimethylformamide / N-methylpyrrolidone mixed solvent (1:1 volume ratio), and then poured into a polytetrafluoroethylene reactor; at 240°C After cooling for 120 min, the reaction solution was centrifuged at 6000 rpm for 10 min to separate the product. The product was washed with a mixed solvent of N,N-dimethylformamide and N-methylpyrrolidone several times and then washed with absolute ethanol. The washed product was finally dried at 60°C for 2 hours to obtain silver sulfide quantum dots. The dried powder was re-dispersed ultrasonically into the above mixed solvent for TEM testing.

[0029] TEM of silver sulfide quantum dots as Figure 4 shown. Figure 4 It shows that the size of the synthesized silver sulfide quantum dots is very small, ranging from 0.9 to 1.9 nm, and the dispersion is very uniform.

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Abstract

The invention discloses a method for preparing ultra-small silver sulfide quantum dots, which is to disperse a single-source precursor in a N,N-dimethylformamide / N-methylpyrrolidone mixed solvent to form a single-source precursor homogeneous solution ; Thermally decompose the single-source precursor homogeneous solution at 210-270°C for 60-120 minutes, after cooling, centrifuge the reaction solution and dry it. The invention synthesizes ultra-small silver sulfide quantum dots through thermal decomposition of a single-source precursor, and effectively regulates the size and size distribution of the silver sulfide quantum dots by controlling the length of the single-source precursor molecule-substituted alkyl chain. The preparation method of the invention is easy to operate and has high reproducibility, and the prepared silver sulfide quantum dots have good crystallinity, small size and uniform size distribution, and good dispersion and dispersion stability.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method of ultra-small silver sulfide quantum dots. Background technique [0002] Quantum dots are quasi-zero-dimensional semiconductor nanomaterials that bind conduction band electrons, valence band holes, and excitons in the three spatial directions of quantum dots, and are composed of a small number of atoms. Generally spherical or quasi-spherical, the size is smaller than or close to the exciton Bohr radius (generally no more than 10nm in diameter), and the movement of electrons in it is restricted in all directions, so it has obvious quantum effects. Due to its small size and special structure, quantum dots exhibit many physical and chemical properties different from macroscopic materials, and have extremely broad application prospects in nonlinear optics, magnetic media, catalysis, medicine, and functional materials. It has a profound i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G5/00C09K11/58B82Y30/00
CPCC01G5/00C09K11/582B82Y30/00C01P2002/72C01P2004/04C01P2004/64
Inventor 马彦军万宏启陈磊冶银平周惠娣陈建敏
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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