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Method for synthesizing size-controllable silver sulfide quantum dots

A synthesis method, silver sulfide technology, applied in chemical instruments and methods, silver compounds, silver compounds, etc., can solve problems such as easy agglomeration, difficulty in controlling particle size, and rapid encounter reaction

Active Publication Date: 2019-04-16
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the ultra-low solubility of Ag2S (Ksp(Ag2S)=6.3×10-50), Ag+ and S2- meet and react quickly, and are easy to agglomerate, the particle size is difficult to control, and the particle size distribution is uneven
Generally, surfactants are introduced in the preparation process to control the agglomeration and size distribution of particles, and the effect is not ideal

Method used

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  • Method for synthesizing size-controllable silver sulfide quantum dots

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1——Synthesis of silver sulfide quantum dots with a particle size of 3nm

[0032] (1) Preparation of silver acetate source solution: 0.1669g silver acetate, first dissolved in oleylamine and then dissolved in 10mL isooctane to obtain a 0.1M silver acetate solution;

[0033] (2) Preparation of sulfur ion-containing inverse microemulsion: 0.2401g Na2S·9H2O was dissolved in 10mL secondary water to obtain a Na2S solution with a concentration of 0.1M. Add 10ml cyclohexane, 1mmol dioctyl sodium succinate sulfonate (concentration is 0.1mol / L) and 0.1mmol co-surfactant n-hexanol to a 25ml brown glass reagent bottle, and make it under magnetic stirring at room temperature Dissolve, add 45 μL of sodium sulfide solution, and 100 Hz ultrasonic for 30 minutes to obtain a reverse microemulsion containing sulfide ions;

[0034] (3) Synthesis of Ag2S quantum dots: Take 45 μL of silver acetate solution, add it to the inverse microemulsion, and ultrasonicate at room temperatur...

Embodiment 2

[0036] Embodiment 2——Synthesis of silver sulfide quantum dots with a particle size of 5nm

[0037] (1) Preparation of silver nitrate source solution: 0.1700g silver nitrate, first dissolved in oleylamine and then dissolved in 10mL isooctane to obtain a 0.1M silver acetate solution;

[0038] (2) Preparation of sulfur ion-containing inverse microemulsion: 0.076 g of thiourea was dissolved in 10 mL of secondary water to obtain a 0.1 M thiourea solution. Add 10ml isooctane, 1mmol dioctyl sodium succinate sulfonate (concentration is 0.1mol / L) and 0.1mmol co-surfactant n-hexanol to a 25ml brown glass reagent bottle, and make it under magnetic stirring at room temperature Dissolve, add 135 μL thiourea solution, and ultrasonicate at 70 Hz for 30 minutes to obtain a reverse microemulsion containing sulfur ions;

[0039](3) Synthesis of Ag2S quantum dots: Take 135 μL of silver nitrate solution and add it to the inverse microemulsion, drop 45 μL each time, once every 10 minutes, and ult...

Embodiment 3

[0041] Embodiment 3——the synthetic process of the silver sulfide quantum dot of 8nm grain size;

[0042] (1) Preparation of silver citrate source solution: 0.171g of silver citrate was first dissolved in oleylamine and then dissolved in 10mL of dodecane to obtain a 0.1M silver citrate solution;

[0043] (2) Preparation of inverse microemulsion containing sulfur ions: 0.075 g of thioacetamide was dissolved in 10 mL of secondary water to obtain a Na2S solution with a concentration of 0.1 M. Add 10ml of dodecane, 1mmol dioctyl sodium succinate sulfonate (concentration is 0.1mol / L) and 0.1mmol co-surfactant n-hexanol to a 25ml brown glass reagent bottle, and make it under magnetic stirring at room temperature Dissolve, add 270 μL of thioacetamide solution, and ultrasonicate at 100 Hz for 30 minutes to obtain a reverse microemulsion containing sulfur ions;

[0044] (3) Synthesis of Ag2S quantum dots: Take 270 μL of silver acetate solution and add it to the inverse microemulsion, d...

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Abstract

The invention discloses a method for synthesizing size-controllable silver sulfide quantum dots, and relates to the technical field of quantum dot material preparation. The method comprises the following steps that 1, under the action of a solvent, a silver source is dissolved in a first alkane solvent, and a solution with the stable silver source is prepared for use; 2, reversed-phase microemulsion is prepared, wherein the reversed-phase microemulsion contains sulfur ions; 3, the silver source solution is added to the reversed-phase microemulsion dropwise, and the silver sulfide quantum dotsare synthesized. The size of the silver sulfide quantum dots is regulated and controlled by adjusting the dosage of the silver ions in the silver source in step 1 and the dosage of the sulfur ions instep 2. The silver sulfide quantum dots prepared through the synthesizing method have size uniformity and size controllability.

Description

technical field [0001] The invention relates to the technical field of preparation of quantum dot materials, in particular to a method for synthesizing size-controllable silver sulfide quantum dots. Background technique [0002] Silver sulfide (Ag2S) quantum dots, a non-toxic semiconductor with a direct narrow bandgap of about 1.0eV, have attracted much attention in the past 10 years. Ag2S quantum dots have unique properties such as wide absorption spectrum, convenient preparation, good chemical stability, and low toxicity, especially because of its excitonic Bohr radius of 2.2 nm, size- and composition-dependent quantum effects, and size-tunable narrow emission. Spectral characteristics have been widely used in photocatalytic degradation of organic pollutants and hydrogen production, quantum dot sensitized solar cells, in vivo and in vitro fluorescence imaging, sensors, etc. [0003] The preparation of size-controllable Ag2S quantum dots has become a research hotspot in re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G5/00B82Y40/00C09K11/58
CPCC01G5/00C01P2004/64C09K11/582
Inventor 刘继宪薛静唐建国王瑶黄林军王薇李海东
Owner QINGDAO UNIV