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Water soluble NaYF4@NaGdF4 nanocrystalline with upconversion core-shell structure and preparation method thereof

A technology of core-shell structure and nanocrystals, which is applied in the field of microwave polyol chemical synthesis, can solve the problems of poor water solubility, low biocompatibility, and low upconversion fluorescence efficiency of particles, and achieve uniform phase, high reaction efficiency, and improved The effect of luminous efficiency

Inactive Publication Date: 2015-04-29
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a rare earth-doped NaYF 4 NaGdF 4 The microwave synthesis and preparation method of up-conversion core-shell structure nanocrystals can solve the problems of poor water solubility of particles, low up-conversion fluorescence efficiency, and low biocompatibility in the existing preparation methods.

Method used

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  • Water soluble NaYF4@NaGdF4 nanocrystalline with upconversion core-shell structure and preparation method thereof
  • Water soluble NaYF4@NaGdF4 nanocrystalline with upconversion core-shell structure and preparation method thereof
  • Water soluble NaYF4@NaGdF4 nanocrystalline with upconversion core-shell structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1NaYF 4 The nucleus is coated with a layer of NaGdF 4 shell

[0057] (1) Mix 2.4mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature for 2h until uniform, and obtain NH 4 F / EG mixed solution.

[0058] (2) Weigh 0.15g of polyethyleneimine into another weighing bottle, add sodium chloride, yttrium trichloride, ytterbium trichloride hexahydrate, and erbium trichloride hexahydrate in proportion; inject 9 mL of ethylene dichloride Alcohol was mixed and stirred to obtain reaction mixture A. Wherein yttrium trichloride and polyethyleneimine are calculated according to the molar ratio of 1:6, and the molar ratio of erbium trichloride hexahydrate, ytterbium trichloride hexahydrate and yttrium trichloride is 2% (ie 0.012mmol): 20% (ie 0.12mmol): 78% (ie 0.468mmol), the total amount of rare earth salt is 0.6mmol; the molar ratio of sodium chloride (0.6mmol) to the total amount of rare earth salt is 1:1.

[0059](3) When the rea...

Embodiment 2

[0065] Example 2NaYF 4 The nucleus is coated with 2 layers of NaGdF 4 shell

[0066] (1) Mix 2.4mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature for 2h until uniform, and obtain NH 4 F / EG mixed solution.

[0067] (2) First weigh 0.15g polyethyleneimine into another weighing bottle, then add sodium chloride, yttrium chloride, ytterbium trichloride hexahydrate, erbium trichloride hexahydrate; Yttrium and polyethyleneimine are calculated at a molar ratio of 1:6, and the molar ratio of erbium trichloride hexahydrate, ytterbium trichloride hexahydrate and yttrium trichloride is 2%:20%:78%; The total amount of rare earth salt is 0.6 mmol, and the molar ratio of sodium chloride to the total amount of rare earth salt is 1:1. In the same weighing bottle, inject 9 mL of ethylene glycol and mix and stir until uniform to obtain reaction mixture A.

[0068] (3) Into the reaction mixture A, quickly inject the prepared ethylene glycol solutio...

Embodiment 3

[0077] Example 3NaYF 4 The nucleus is coated with 3 layers of NaGdF 4 shell

[0078] (1) Mix 2.4mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature for 2h until uniform, and obtain NH 4 F / EG mixed solution.

[0079] (2) First weigh 0.15g polyethyleneimine into another weighing bottle, then add sodium chloride, yttrium chloride, ytterbium trichloride hexahydrate, erbium trichloride hexahydrate; Yttrium and polyethyleneimine are calculated at a molar ratio of 1:6, and the molar ratio of erbium trichloride hexahydrate, ytterbium trichloride hexahydrate and yttrium trichloride is 2%:20%:78%; The total amount of rare earth salt is 0.6 mmol, and the molar ratio of sodium chloride to the total amount of rare earth salt is 1:1. In the same weighing bottle, inject 9 mL of ethylene glycol and mix and stir until uniform to obtain reaction mixture A.

[0080] (3) Into the reaction mixture A, quickly inject the prepared ethylene glycol solutio...

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Abstract

The invention relates to a water soluble NaYF4@NaGdF4 nanocrystalline with an upconversion core-shell structure and a preparation method thereof, and belongs to the technical field of microwave polyhydric alcohol chemical method synthesis. The nanocrystalline with the upconversion core-shell structure provided by the invention, is regulatable balls with different sizes in addition amount of an outer polytetrafluorogadolinium sodium shell, and the average diameter is 14-38 nanometers. The physical phase is converted from square phase to hexagonal phase. According to the nanocrystalline with the core-shell structure provided by the invention, polyethyleneimine covers the surface of the polytetrafluorogadolinium sodium nanocrystalline, so that the particles have good water solubility, and the shape of products can be controlled, and the nanocrystalline has good biological compatibility. Along with increase of the shell layer, upconversion luminescence is increased, and the fluorescent lifetime cancellation time is prolonged. The nanocrystalline can be used as an effective CT (Computed Tomography) responder and has potential application value in the fields such as biological imaging. The nanocrystalline with the core-shell structure has higher fluorescence efficiency and better water solubility and biological application value.

Description

technical field [0001] The invention belongs to the field of microwave polyol chemical synthesis technology, in particular to a preparation method of water-soluble up-conversion core-shell fluorescent nanocrystals. Background technique [0002] An up-conversion material is a luminescent material that is excited by a long wavelength and emits short-wavelength light, that is, a material that converts low-energy photons into high-energy photons. Up-conversion luminescence imaging uses near-infrared (such as 980nm) continuous laser excitation, which has relatively low tissue absorption and scattering, and can completely eliminate biological background fluorescence. In addition, rare earth-doped fluoride nanocrystals have low phonon energy, low toxicity, good chemical stability, large Stokes shift and narrow and strong emission peaks with long fluorescence lifetime, deep tissue penetration depth and infrared excitation The advantage of being easy, is widely used in related cutti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85C09K11/02
Inventor 施展李菲菲李春光白天语陈彩玲冯守华
Owner JILIN UNIV
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