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Synthesis method of near infrared silver sulfide quantum dots

A synthesis method and technology of silver sulfide, applied in the direction of chemical instruments and methods, pharmaceutical formulations, preparations for in vivo tests, etc., can solve the problems of simple, green, high-yield, high-efficiency, increase the difficulty of synthesis of silver sulfide quantum dots, Problems such as changes in the original properties of quantum dots, to achieve the effect of simple green synthesis, good biocompatibility, and stable optical properties

Inactive Publication Date: 2017-12-01
NORTHEASTERN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

In aqueous phase synthesis, the nucleation process of silver sulfide is affected by many factors, such as the concentration of reactants, the temperature and time of nucleation, the speed of reactant addition, etc. These precise and complex adjustments increase the quantum of silver sulfide. The synthesis difficulty of points does not conform to the principle of "simple, green, high-yield, and efficient", which is not conducive to the promotion in practical applications
The traditional method of synthesizing near-infrared silver sulfide quantum dots in the organic phase is often accompanied by high-temperature and high-heat reactions, and it needs to be converted into the aqueous phase through ligand exchange after the synthesis. However, incomplete ligand exchange often occurs during the conversion process. , the surface structure of quantum dots changes, the aggregation of quantum dots precipitates or the particle size increases, resulting in changes in the original properties of quantum dots

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  • Synthesis method of near infrared silver sulfide quantum dots
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  • Synthesis method of near infrared silver sulfide quantum dots

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[0042] The invention provides a kind of synthetic method of near-infrared silver sulfide quantum dot, and described synthetic method comprises the following steps:

[0043] 1) Dissolve the silver nitrate crystals in the polar solvent ethylene glycol, and stir until dissolved at 3°C-5°C in the dark to obtain solution A;

[0044] 2) In the state of stirring, add mercaptocarboxylic acid solution to obtain solution B;

[0045] 3) Place the solution B under the condition of 70°C-80°C in the dark and stir, and react for 2min-8min, the solution B gradually turns from colorless to milky white, gradually forming silver sulfide crystal nuclei;

[0046] 4) Increase the reaction temperature from 70°C-80°C to 140°C-150°C, continue the reaction, the solution B gradually changes from milky white to clear brown, forming a stable silver sulfide crystal nucleus;

[0047] 5) rapidly cool to room temperature, terminate the reaction;

[0048] 6) Ultrafiltration to remove the solvent and reaction...

Embodiment 1

[0061] Embodiment 1 proposes a kind of synthetic method of near infrared silver sulfide quantum dot, comprises the following steps:

[0062] 1) Weigh 8.49 mg (0.05 mmol) of silver nitrate crystals and dissolve them in 20 ml of anhydrous ethylene glycol, and stir at 4°C in the dark until the silver nitrate dissolves to obtain 2.5 mmol / L silver nitrate solution A;

[0063] 2) Slowly add 0.05 mmol of 3-mercaptopropionic acid to solution A under stirring to obtain colorless and transparent solution B;

[0064] 3) Put solution B in an oil bath at 75°C, stir evenly for 5 minutes, solution B gradually changes from colorless to milky white;

[0065] 4) At a heating rate of 10°C / min, raise the temperature of the oil bath reaction system from 75°C to 145°C in about 7 minutes, start timing when the temperature reaches 145°C, and continue the reaction for 100 minutes to obtain a clear and translucent brown reaction solution ;

[0066] 5) Rapidly cool down to room temperature in an ice b...

Embodiment 2-3

[0072] Embodiment 2-3 proposes a kind of synthetic method of near-infrared silver sulfide quantum dots respectively, and synthetic procedure is the same as embodiment 1, and difference is: the amount of adding 3-mercaptopropionic acid in step 2) is respectively: 0.075mmol, 0.1 mmol, that is, the feeding ratio of silver nitrate / 3-mercaptopropionic acid is 1:1.5, 1:2 respectively.

[0073] The average particle size, average surface potential and fluorescence emission range of silver sulfide quantum dots obtained in Examples 2-3 are shown in Table 1.

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Abstract

The invention discloses a synthesis method of near infrared silver sulfide quantum dots, belonging to the technical field of functional nanomaterials. The synthesis method comprises the following steps: (1) dissolving silver nitrate crystals into a polar solvent ethylene glycol, stirring at a dark place being 3 DEG C-5 DEG C until dissolving is achieved, so as to obtain a solution A; (2) under the stirring state, adding a mercaptan carboxylic acid solution to obtain a solution B; (3) placing the solution B under the condition of 70 DEG C to 80 DEG C and stirring at a dark place, reacting for 2min to 8min, so as to lead the solution B to gradually become milk white from colorless and gradually form silver sulfide crystal nucleus; (4) increasing the reaction temperature to 140 DEG C to 150 DEG C from 70 DEG C to 80 DEG C, continuously reacting, to gradually transform the milk white solution B into clear brown solution B, and form stable silver sulfide crystal nucleus; (5) rapidly cooling to room temperature and stopping reaction; and (6) ultrafiltering to remove the solvent and reaction side products, adding water for washing and dispersing, to obtain silver sulfide quantum dots. The method is simple and highly efficient, and can conduct mass production, the synthesized quantum dots are good in water phase dispersity, scattered and uniform in particle size and stable in optical property.

Description

technical field [0001] The invention belongs to the technical field of functional nanometer materials, and relates to a method for synthesizing carboxyl water-soluble silver sulfide quantum dots with near-infrared fluorescence properties. Background technique [0002] Quantum dots are microcrystalline particles with a particle size distribution of 1-100nm, because of their unique physical and chemical properties, such as quantum size effects, dielectric confinement effects, etc., which make the energy band of quantum dots become molecular or The separated energy level structure of atomic characteristics shows many characteristics superior to those of bulk materials, so it has great application value in the fields of biomedicine and molecular imaging. [0003] Silver sulfide quantum dots, as a nano-semiconductor material with high biocompatibility, have attracted much attention in recent years. Its optical properties are stable, the fluorescence spectrum can be adjusted, and ...

Claims

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Application Information

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IPC IPC(8): C09K11/58B82Y20/00B82Y40/00A61K49/00
CPCC09K11/582A61K49/0067B82Y20/00B82Y40/00
Inventor 刘弘光张营程震
Owner NORTHEASTERN UNIV
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