A method for preparing size-controllable organic phase silver selenide quantum dots

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

Active Publication Date: 2022-04-22
WUHAN UNIV
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  • 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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  • A method for preparing size-controllable organic phase silver selenide quantum dots
  • A method for preparing size-controllable organic phase silver selenide quantum dots
  • A method for preparing size-controllable organic phase silver selenide quantum dots

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Embodiment 1

[0035] 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

[0037] 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-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 te...

Embodiment 3

[0039]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, which comprises the following steps: mixing a silver source, a solvent and a surface ligand at room temperature under stirring conditions, and introducing a protective gas to obtain a silver precursor Mix selenium powder and oleylamine at room temperature and under ultrasonic conditions to obtain a selenium precursor; raise the temperature of the above silver precursor to 120-180°C, add the selenium precursor, and react at 100-150°C for a period of time, then drop to room temperature, Ag was obtained through separation and purification 2 Se quantum dots. with existing Ag 2 Compared with Se quantum dot synthesis method, the Ag provided by the invention 2 The synthesis method of Se quantum dots mainly has the following two advantages: first, the preparation of the selenium precursor is simple, and only need to ultrasonicate the selenium powder and oleylamine at room temperature; 2 The fluorescence emission peak of Se quantum dots is adjustable in the range of 955nm to 1612nm. Ag prepared by the present invention 2 Se quantum dots have good monodispersity and tunable wavelength in the near-infrared region, and have potential applications in the fields of biomedicine and material science.

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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Patent Type & Authority Patents(China)
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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