Quantum dot fluorescent nanosphere based on amphiphilic silicon carrier, and preparation method thereof

A fluorescent nanometer and quantum dot technology, which is applied in nanotechnology, nanotechnology, nano-optics, etc. for materials and surface science, can solve the cumbersome preparation process of quantum dot fluorescent nanospheres, poor controllability of size and particle size distribution, Fluorescence intensity is easy to lose and other problems, to achieve the effects of controllable quantum dot coating amount and size, scaling size, quantum dot coating amount, and regular shape

Active Publication Date: 2020-02-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the cumbersome preparation process of the existing quantum dot fluorescent nanospheres and the easy loss of fluorescence intensity, the present invention provides an amphiphilic silicon carrier with regular shape, controllable quantum dot coating amount and size, high luminescence and stable performance. quantum dot fluorescent nanosphere
[0007] The invention aims to overcome the poor controllability of the size and particle size distribution of the microspheres existing in the existing synthesis process of quantum dot fluorescent nanospheres, ligand replacement on the surface of quantum dots during the phase inversion process, and fluorescence intensity easily caused by by-products or additives. For the problem of serious loss, a preparation method of quantum dot fluorescent nanospheres based on amphiphilic silicon carrier is provided. This method uses the amphiphilic carrier formed by the hydrolysis and condensation of hydrophobic silane precursors to directly and efficiently water-soluble Modification, the size of nanospheres and the coating amount of quantum dots can be effectively scaled by simply adjusting the concentration of quantum dots

Method used

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  • Quantum dot fluorescent nanosphere based on amphiphilic silicon carrier, and preparation method thereof
  • Quantum dot fluorescent nanosphere based on amphiphilic silicon carrier, and preparation method thereof
  • Quantum dot fluorescent nanosphere based on amphiphilic silicon carrier, and preparation method thereof

Examples

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Effect test

Embodiment 1

[0040] (1) Take 750 μL of cadmium selenide / zinc sulfide quantum dot stock solution (2.1×10 - 5 mol / L), an equal volume of methanol was added to precipitate quantum dots. Discard the supernatant after centrifugation, dry the precipitate slightly in the air, then add 40 μL of n-octyltriethoxysilane, and fully dissolve to obtain an orange transparent solution, which is the quantum dot-organosilane precursor;

[0041] (2) Transfer the quantum dot-organosilane precursor to a glass bottle, add 40mL water and 60μL ammonia water (28wt%); extend the ultrasonic probe (diameter 6mm) below the liquid surface, set the amplitude to 30%, and 5s ultrasonication / 3s pause is the working cycle, ultrasonic treatment for 1h, to obtain quantum dot micellar solution;

[0042] (3) Filter the quantum dot micellar solution through a 0.22 μm microporous membrane, add 1.6 mL of sodium silicate solution (0.54 wt%), stir and react for 24 hours, and prepare CdSe / ZnS@SiO with a diameter of 25 nm 2 Crude s...

Embodiment 2

[0045] The difference between Example 2 and Example 1 is that step (4) is added: use an ultrafiltration centrifuge tube to concentrate the above-mentioned CdSe / ZnS@SiO 2 A crude solution of fluorescent nanospheres until the absorbance of the quantum dots (at the position of its exciton absorption peak) reaches about 0.1. Then, 3 mL of the above solution was added to 12 mL of ethanol, 0.2 mL of ammonia water and 15 μL of tetraethyl orthosilicate mixed solution, slowly stirred and reacted for 6 hours to coat the silica layer, and the CdSe / ZnS@ SiO 2 Quantum dot fluorescent nanospheres.

[0046] image 3 It is CdSe / ZnS@SiO after oil-soluble cadmium selenide / zinc sulfide quantum dots (a) and the grown silica shell layer obtained in Example 2 2 The transmission electron microscope image of quantum dot fluorescent nanospheres (b), it can be seen that the oil-soluble cadmium selenide / zinc sulfide quantum dots with uniform particle size and good monodispersity are modified by amphi...

Embodiment 3

[0048] (1) Take 400 μL of cadmium selenide / zinc sulfide quantum dot stock solution (2.1×10 - 5 mol / L), an equal volume of methanol was added to precipitate quantum dots. Discard the supernatant after centrifugation, dry the precipitate slightly in the air, then add 40 μL of n-octyltriethoxysilane, and fully dissolve to obtain an orange transparent solution, which is the quantum dot-organosilane precursor;

[0049] (2) Transfer the quantum dot-organosilane precursor to a glass bottle, add 40 mL of water and 60 μL of ammonia water (28 wt%). Extend the ultrasonic probe (diameter 6mm) below the liquid surface, set the amplitude to 30%, use 5s ultrasonication / 3s pause as the working cycle, and ultrasonically treat for 1h to obtain the quantum dot micellar solution;

[0050] (3) Filter the quantum dot micellar solution through a 0.22μm microporous membrane, add 1.6mL sodium silicate solution (0.54wt%), stir and react for 24h, and obtain CdSe / ZnS@SiO with a diameter of 16nm 2 crud...

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Abstract

The invention relates to the technical field of fluorescent nanometer materials. In order to solve the problems of tedious preparation process and easy fluorescence intensity loss of the existing quantum dot fluorescent nanospheres, the invention provides a quantum dot fluorescent nanosphere based on an amphiphilic silicon carrier, and a preparation method thereof, wherein the quantum dot fluorescent nanosphere based on the amphiphilic silicon carrier is formed by coating the surface of hexadecylamine and trioctylphosphine oxide co-modified cadmium selenide/zinc sulfide quantum dot with a silicon dioxide layer. According to the invention, the quantum dot fluorescent nanosphere is regular in form, controllable in quantum dot coating amount and size, high in luminescence and stable in performance; and the preparation method is simple, wherein the size of the nanospheres and the coating amount of the quantum dots can be effectively reduced and increased by adjusting the concentration of the quantum dots, and the more surface functional modification and assembly are expected to be achieved through the controllable silicon dioxide shell growth.

Description

technical field [0001] The invention relates to the technical field of fluorescent nanomaterials, in particular to a quantum dot fluorescent nanosphere based on an oil-phase quantum dot and an amphiphilic silicon carrier and a preparation method thereof. Background technique [0002] As a new nanoluminescent material, quantum dots (QDs) have the characteristics of high luminous intensity, wavelength tunability, anti-photobleaching and high color purity, and have a wide range of applications in the fields of high-sensitivity biosensing, multivariate analysis, and multimodal imaging. . At present, the synthesis methods of quantum dots are mainly divided into two categories: aqueous phase synthesis and organic phase synthesis. Water-soluble quantum dots have advantages in biocompatibility, but their quantum efficiency is low, their fluorescence stability is generally poor, and their particle size distribution is wide. The oil-soluble quantum dots synthesized by the organic ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/88B82Y20/00B82Y30/00
CPCC09K11/025C09K11/883B82Y20/00B82Y30/00
Inventor 黄亮金洁宁胡军汪晶
Owner ZHEJIANG UNIV OF TECH
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