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Preparation method for fluorescent silver sulfide quantum dots in near-infrared-II region and silver sulfide quantum dots

A technology of silver sulfide and quantum dots, applied in chemical instruments and methods, silver compounds, silver compounds, etc., can solve problems such as complex preparation process, and achieve uniform particle size, good fluorescent properties, and low biological toxicity

Inactive Publication Date: 2020-01-24
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is relatively little work related to the synthesis of fluorescent silver sulfide quantum dots, and the silver precursors used in most methods need to be synthesized separately, and the entire preparation process is relatively complicated.

Method used

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  • Preparation method for fluorescent silver sulfide quantum dots in near-infrared-II region and silver sulfide quantum dots
  • Preparation method for fluorescent silver sulfide quantum dots in near-infrared-II region and silver sulfide quantum dots
  • Preparation method for fluorescent silver sulfide quantum dots in near-infrared-II region and silver sulfide quantum dots

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preparation example Construction

[0032] see Figure 1 to Figure 8 As shown, a preparation method of near-infrared second-region fluorescent silver sulfide quantum dots includes the following steps:

[0033] S1, a preset amount of silver acetylacetonate is added to the solution of alkyl mercaptan to obtain reaction solution;

[0034] S2, heating the reaction solution to a preset temperature under nitrogen protection, and continuing to react for a preset time at the preset temperature;

[0035] S3, the reaction solution is naturally cooled to 50°C under stirring;

[0036] S4, add ethanol to reaction solution, carry out sedimentation;

[0037] S5, performing centrifugal washing treatment;

[0038] S6, adding chloroform to the reaction solution to obtain a solution of silver sulfide fluorescent quantum dots dispersed in chloroform.

Embodiment 1

[0042] 2) Under nitrogen protection, the reaction solution was gradually heated to 190°C and maintained for 10min;

[0043] 3) Naturally cooling the reaction solution to 50°C under stirring;

[0044] 4) add ethanol to reaction solution, carry out sedimentation;

[0045] 5) carry out centrifugal washing treatment;

[0046] 6) adding chloroform to the reaction solution to obtain a solution of silver sulfide fluorescent quantum dots dispersed in chloroform.

[0047] The experimental results show that, see figure 2 and combine Image 6 As shown in the fluorescence emission spectrum 10 of the silver sulfide quantum dots prepared in this example, the prepared silver sulfide quantum dots have a spherical shape of about 5.8 ± 0.8 nm, and the fluorescence intensity is high, but the dispersion is poor from the projection electron microscope. , the agglomeration phenomenon is serious.

Embodiment 2

[0049] 1) 51mg silver acetylacetonate is added in 20ml n-octadecanethiol to obtain reaction solution;

[0050] 2) Under nitrogen protection, the reaction solution was gradually heated to 190°C and maintained for 10min;

[0051] 3) Naturally cooling the reaction solution to 50°C under stirring;

[0052] 4) add ethanol to reaction solution, carry out sedimentation;

[0053] 5) carry out centrifugal washing treatment;

[0054] 6) adding chloroform to the reaction solution to obtain a solution of silver sulfide fluorescent quantum dots dispersed in chloroform.

[0055] The experimental results show that when n-octadecanethiol is used as the sulfur precursor, the particle size of the prepared silver sulfide quantum dots is small, about 4.0±0.5nm, with certain agglomeration and relatively low fluorescence intensity.

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Abstract

The invention discloses a preparation method for fluorescent silver sulfide quantum dots in a near-infrared-II region. The method includes the following steps: S1, adding a preset amount of silver(I)2,4-pentanedionate into an alkyl mercaptan solution; S2, heating the reaction solution to a preset temperature under the protection of nitrogen, and maintaining the preset temperature for a preset time; S3, naturally cooling the reaction solution to 50 DEG C under stirring; S4, performing precipitation by using ethanol; S5, performing centrifugal washing treatment; and S6, adding chloroform into the reaction solution to obtain the silver sulfide fluorescent quantum dot solution dispersed in the chloroform. The silver sulfide quantum dots prepared by the method have a uniform particle size, have good fluorescence properties in the near-infrared-II region, can be connected with a hydrophilic ligand through a ligand exchange reaction to be converted into an aqueous phase, have low biologicaltoxicity, and can be used for biomedical imaging and construction of biological fluorescent probes.

Description

technical field [0001] The invention relates to the technical field of nano-composite materials, in particular to a preparation method of near-infrared second-region fluorescent silver sulfide quantum dots and the silver sulfide quantum dots prepared by the method. Background technique [0002] Due to the low scattering and good penetration depth of long-wavelength light in living tissue, NIR II (1000-1700 nm) imaging has obvious advantages over traditional NIR I (650-950 nm) imaging in in vivo imaging , which can obtain higher-resolution images, thus becoming one of the hot spots in the field of optical imaging. [0003] Silver sulfide is a kind of semiconductor material of I-VI group with high chemical stability and narrow energy band. It has good photoelectric and thermoelectric properties. It has been widely used in photovoltaic cells, infrared detectors and other fields. Nanoscale silver sulfide particles have tunable fluorescence properties in the near-infrared region...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/58C01G5/00B82Y20/00B82Y40/00
CPCC09K11/582C01G5/00B82Y20/00B82Y40/00
Inventor 陆峰范曲立张凯威程威王其黄维
Owner NANJING UNIV OF POSTS & TELECOMM