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Method for preparing organic-phase silver selenide quantum dots with controllable sizes

A quantum dot and organic phase technology, which is applied in the field of preparation of size-controllable organic phase silver selenide quantum dots, can solve the problems of narrow control range of quantum dot size, uncontrollable fluorescence emission peak, complex preparation of selenium precursors, etc., to achieve Low price of raw materials, conducive to industrial production and promotion, low price effect

Active Publication Date: 2020-01-31
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the above-mentioned technical problems, the present invention provides an Ag with simple preparation and wide range of size control. 2 The synthesis method of Se quantum dots aims to solve the complex preparation of selenium precursors in the prior art or involve expensive and toxic phosphorus-containing reagents, and Ag 2 The size control range of Se quantum dots is narrow, and the fluorescence emission peak cannot be adjusted to the NIR-IIb region

Method used

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  • Method for preparing organic-phase silver selenide quantum dots with controllable sizes
  • Method for preparing organic-phase silver selenide quantum dots with controllable sizes
  • Method for preparing organic-phase silver selenide quantum dots with controllable sizes

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Embodiment 1

[0037] Add 1mmol of silver acetate, 10mmol of n-octyl mercaptan, and 10mL of 1-octadecene into a three-necked flask equipped with a thermometer and a condenser tube. Under stirring conditions, pass argon under the liquid surface and heat to 120°C; until completely dissolved After that, change to the liquid surface to ventilate and continue to heat up. At the same time, 0.1mmol selenium powder, 0.8mL oleylamine, and 1.1mL 1-octadecene were mixed and ultrasonicated to obtain a selenium precursor. When the temperature rose to 160°C, the above-mentioned selenium precursor was quickly injected into the three-neck flask with a syringe, the temperature was lowered to 120°C, and the temperature was kept for 10 minutes. Cool down to room temperature, add 10 mL of acetonitrile and 50 mL of acetone, centrifuge at 10,000 rpm for 5 min, discard the supernatant to obtain a precipitate, and then purify twice through tetrachlorethylene dispersion of acetonitrile plus acetone precipitation ste...

Embodiment 2

[0039] Add 0.9mmol of silver acetate, 10mmol of n-octyl mercaptan, and 10mL of 1-octadecene into a three-necked flask equipped with a thermometer and a condenser tube, and heat to 120°C with argon under the liquid surface under stirring conditions; After dissolving, change to the liquid surface to ventilate, and continue to heat up. At the same time, 0.1mmol selenium powder, 0.8mL oleylamine, and 1.1mL 1-octadecene were mixed and ultrasonicated to obtain a selenium precursor. When the temperature rose to 160°C, the above-mentioned selenium precursor was quickly injected into the three-neck flask with a syringe, the temperature was lowered to 120°C, and the temperature was kept for 10 minutes. Cool down to room temperature, add 10 mL of acetonitrile and 50 mL of acetone, centrifuge at 10,000 rpm for 5 min, discard the supernatant to obtain a precipitate, and then purify twice through tetrachlorethylene dispersion of acetonitrile plus acetone precipitation steps, disperse in tet...

Embodiment 3

[0041]Add 0.55mmol of silver acetate, 10mmol of n-octyl mercaptan, and 10mL of 1-octadecene into a three-necked flask equipped with a thermometer and a condenser tube. Under stirring conditions, pass argon under the liquid surface and heat to 120°C; After dissolving, change to the liquid surface to ventilate, and continue to heat up. At the same time, 0.1mmol selenium powder, 0.8mL oleylamine, and 1.1mL 1-octadecene were mixed and ultrasonicated to obtain a selenium precursor. When the temperature rose to 170°C, the above-mentioned selenium precursor was quickly injected into the three-necked flask with a syringe, the temperature was lowered to 120°C, and the temperature was kept for 10 minutes. Cool down to room temperature, add 10 mL of acetonitrile and 50 mL of acetone, centrifuge at 10,000 rpm for 5 min, discard the supernatant to obtain a precipitate, and then purify twice through tetrachlorethylene dispersion of acetonitrile plus acetone precipitation steps, disperse in ...

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Abstract

The invention discloses a method for preparing size-controllable organic-phase silver selenide quantum dots. The method comprises the following steps: mixing a silver source, a solvent and a surface ligand at room temperature under stirring conditions, and introducing protective gas to obtain a silver precursor; and mixing selenium powder and fatty amine at room temperature under ultrasonic conditions to obtain a selenium precursor; and heating the silver precursor to 120-180 DEG C, adding a selenium precursor, carrying out a reaction at 100-150 DEG C for a period of time, then performing cooling to room temperature, and carrying out separating and purifying to obtain the Ag2Se quantum dots. Compared with conventional Ag2Se quantum dot synthesis methods, the Ag2Se quantum dot preparation method provided by the invention mainly has the following two advantages: 1, the selenium precursor is simple to prepare, and is prepared by only subjecting selenium powder and fatty amine to ultrasonic treatment at room temperature; and 2, the size adjustable range is wide, and the fluorescence emission peak of the Ag2Se quantum dots can be adjusted within the range of 955 nm to 1612 nm. The Ag2Sequantum dots prepared by the method are good in monodispersity; the wavelength of the Ag2Se quantum dots is adjustable in a near-infrared region; and the Ag2Se quantum dots have application potentialin the fields of biomedicine, material science and the like.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing size-controllable organic phase silver selenide quantum dots. Background technique [0002] Living tissues and organs have lower autofluorescence and better penetration depth in the near-infrared long wavelength range (NIR-IIb, 1500nm-1700nm). Therefore, fluorescent materials with emission wavelengths in this range have good application potential in the field of in vivo imaging. Quantum dots are ideal fluorescent materials due to their excellent optical properties. However, at present, the quantum dots whose wavelength can be adjusted to the NIR-IIb region are mainly lead-containing quantum dots, and the potential toxicity of lead greatly limits the application prospects of lead-containing quantum dots in the field of biological imaging. Therefore, the development of new lead-free near-infrared quantum dots Quantum dots became...

Claims

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Application Information

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IPC IPC(8): C09K11/88B82Y20/00B82Y40/00
CPCC09K11/881B82Y20/00B82Y40/00
Inventor 庞代文刘振亚田智全刘安安
Owner WUHAN UNIV
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