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Core-shell zinc oxide-silica nanoparticle, and preparation method and application thereof

A technology of zinc oxide nanoparticles and nanoparticles, which is applied in the field of nanomaterials, can solve the problems of large particle size, unsatisfactory products, and application limitations of bioluminescence labeling, etc., and achieve the effect of mild reaction conditions

Inactive Publication Date: 2012-10-17
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the visible emission mechanism of ZnO is surface defect light emission, it is easily affected by the external environment, water, weak acid, weak base, etc. will cause fluorescence quenching, and the quantum yield of ZnO quantum dots synthesized by traditional methods is generally lower than 10%, making its application of bioluminescence labeling limited
Researchers try to adjust various conditions to increase the quantum yield of ZnO, such as replacing the reaction raw material zinc salt or alkali, or using different coating methods to protect its surface defects, such as coating with polymers and organic silicon. However, so far, the researched products are still unsatisfactory. For example, the coating protection effect is not significant, the coating process leads to a significant reduction in the quantum yield of ZnO quantum dots, or the obtained product particle size is too large, which is a shell layer. Coated multi-core structures, etc.

Method used

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  • Core-shell zinc oxide-silica nanoparticle, and preparation method and application thereof
  • Core-shell zinc oxide-silica nanoparticle, and preparation method and application thereof
  • Core-shell zinc oxide-silica nanoparticle, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of ethanol solution of zinc oxide nanoparticles

[0028] Dissolve 2.35 g of zinc methacrylate in 100 ml of absolute ethanol, stir and heat to 80 o C, reflux for 1 hour; dissolve 1.26 g of lithium hydroxide monohydrate in 100 ml of absolute ethanol, and use ultrasound to help dissolve. Then the ethanol solution of zinc methacrylate and the ethanol solution of lithium hydroxide were mixed, stirred at room temperature and reacted for 24 hours, then 40 o C was concentrated by rotary evaporation, added ethyl acetate to precipitate, centrifuged at 5000 rpm for 5 minutes, discarded the supernatant, and dissolved the precipitate with 200 ml of absolute ethanol (precipitation mass 0.32-0.4 g). The resulting ethanol solution was designated as ZnO-A.

[0029] (2) Preparation of ethanol solution of zinc oxide nanoparticles coated with organic silicon monolayer

[0030] Take 50 ml of ZnO-A solution (zinc oxide nanoparticles 0.08-0.1 g) and add 50 ml of absolute et...

Embodiment 2

[0038] The preparation method is the same as in Example 1, but the lithium hydroxide monohydrate used in the step (1) is 0.63g, and the hydrolysis rate of the zinc salt slows down under this condition, and finally the ZnO average diameter obtained is 3.8 nanometers (attached figure 2 ), its aqueous solution is denoted as ZnO-BSiO 2 . Its luminous wavelength is around 513 nanometers, and its quantum efficiency is about 48%. It can emit stably in both phosphate buffer and RPMI 1640 medium.

[0039] The cell culture and test process were the same as in Example 1. The semi-lethal concentration of human cervical cancer cell Hela is about 0.3mg / mL, and the ZnO quantum dots can enter the cytoplasm, but it is not obvious in the nucleus. The experimental results show that the ZnO nanoparticle quantum dots in the present invention have good Cell compatibility, and in cells, it can stably emit light under continuous ultraviolet excitation.

Embodiment 3

[0041] The preparation method is the same as that in Example 1, but the lithium hydroxide monohydrate used in step (1) is 0.63 g, and the stirring time at room temperature after mixing zinc methacrylate and lithium hydroxide ethanol solution in step (1) is 20 days. Under this condition, the average diameter of ZnO finally obtained is 4.6 nm (attached image 3 ), and its aqueous solution is denoted as ZnO-CSiO 2 . Its luminous wavelength is around 550 nm, and its quantum efficiency is about 33%. It can emit stably in both phosphate buffer and RPMI 1640 medium.

[0042] The cell culture and test process were the same as in Example 1. The semi-lethal concentration for human cervical cancer cell Hela was about 0.2 mg / mL. The ZnO quantum dots could all enter the cytoplasm, but it was not obvious in the nucleus. The experimental results showed that this The ZnO nanoparticle quantum dots in the invention have good cell compatibility, and can stably emit light under continuous ultra...

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Abstract

The invention specifically relates to a core-shell zinc oxide-silica nanoparticle, and a preparation method and application thereof, belonging to the technical field of nano-materials. The method comprises the following steps: subjecting lithium hydroxide and zinc methacrylate to hydrolysis at room temperature to produce luminous ZnO nanoparticles, adding siloxane monomers containing double bonds and azodiisobutyronitrile, carrying out heating to initiate polymerization so as to form a single organosilicon layer on the surface of the ZnO nanoparticles, then adding other siloxane and ammonia water, and carrying out hydrolysis at room temperature to form a silicon dioxide layer so as to prepare the core-shell zinc oxide-silica nanoparticles. The core of a core-shell zinc oxide-silica nanoparticle is a single zinc oxide luminous quantum dot and has a diameter of 2.7 to 4.6 nm; the shell of the nanoparticle is a thin silica layer; and the core-shell zinc oxide-silica nanoparticle is safe and nontoxic, has high quantum efficiency, stably emits light under continuous UV excitation in cells, can be used for preparing fluorescent labels for biological cells and is especially applicable to preparation of fluorescent labels for cervical carcinoma cells.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and specifically relates to a core-shell type "zinc oxide-silicon dioxide" nanoparticle and its preparation method and application. Background technique [0002] Since the 1990s, scientists have recognized the application prospects of semiconductor luminescent quantum dots as bioluminescent markers, especially the research on the intersection of luminescent nanocrystals and biomedicine has aroused great interest of scientists and achieved remarkable results. . [0003] Semiconductor luminescent quantum dots have incomparable advantages over organic dyes in the application of bioluminescent labeling. For example, the fluorescent color of quantum dots can be adjusted by controlling their composition and particle size; the excitation peak of quantum dots is wide and the emission peak is narrow, symmetrical. Gaussian distribution, small overlap, so the same excitation light can be used t...

Claims

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Application Information

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IPC IPC(8): C09K11/59C12Q1/02G01N21/64
Inventor 张华娟熊焕明任庆广
Owner FUDAN UNIV
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