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Preparation method of water-soluble upconversion fluorescence nano material

A fluorescent nanomaterial, water-soluble technology, applied in the direction of luminescent materials, nanotechnology, nano-optics, etc., can solve the problems of unsuitability for biological analysis, complicated pretreatment operation, large size, etc., to achieve a safe and non-toxic reaction process, suitable for The effect of mass production and uniform size distribution

Inactive Publication Date: 2013-12-25
GUANGZHOU IMPROVE MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The hexagonal phase up-conversion fluorescent nanomaterials prepared by the existing methods are all oil-soluble. To be used in biomarkers, the oil-soluble up-converting fluorescent nanomaterials must be prepared by ligand exchange, ligand oxidation, layer-by-layer assembly and surface silanization. The conversion of fluorescent nanomaterials into water-soluble ones requires complex pretreatment operations, and the water solubility is not easy to control; while water-soluble up-conversion fluorescent nanomaterials are mostly cubic crystal phases or mixed with a small proportion of hexagonal crystal phases. Crystal phase, low up-conversion luminescence intensity, and large size, not suitable for biological analysis
In the current preparation methods of water-soluble upconversion fluorescent nanomaterials, the crystal phase, size and water solubility of crystals cannot be balanced, which greatly affects their application as biomarker materials.

Method used

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  • Preparation method of water-soluble upconversion fluorescence nano material
  • Preparation method of water-soluble upconversion fluorescence nano material
  • Preparation method of water-soluble upconversion fluorescence nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 2ml of rare earth nitrate solution (the mass of rare earth nitrate is 0.1458g, and the molar ratio of each rare earth ion is yttrium ion:ytterbium ion:erbium ion=80:18:2), add 12ml of absolute ethanol to it, and then add 0.9000 g polyacrylic acid (the mass ratio of rare earth nitrate to polyacrylic acid is 0.162:1) aqueous solution 14ml, stirred for 10min; then add 0.2100g sodium fluoride (F - / Ln 3+ Molar ratio of 10:1) aqueous solution 8ml, after stirring for 20min, put it in a high-pressure reactor, and react at 200°C for 10h under stirring condition; stop heating and keep stirring to cool to room temperature, centrifuge to separate the solid product, and use anhydrous Wash with ethanol and ultrapure water three times respectively, and vacuum-dry at room temperature for 12 hours to obtain a solid upconversion fluorescent material, and its X-ray diffraction spectrum (XRD) and transmission electron microscope (TEM) are as follows: figure 1 shown; figure 1 The X-...

Embodiment 2

[0038] Take 2ml of rare earth nitrate solution (the mass of rare earth nitrate is 0.1458g, and the molar ratio of each rare earth ion is yttrium ion:ytterbium ion:erbium ion=80:18:2), add 18ml of absolute ethanol to it, and then add 0.9000 8ml of an aqueous solution of polyacrylic acid (the mass ratio of rare earth nitrate to polyacrylic acid is 0.162:1), stirred for 10min; then add 0.2100g of sodium fluoride (F - / Ln 3+ Molar ratio of 10:1) aqueous solution 8ml, after stirring for 20min, put it in a high-pressure reactor, and react at 200°C for 10h under stirring condition; stop heating and keep stirring to cool to room temperature, centrifuge to separate the solid product, and use anhydrous Wash with ethanol and ultrapure water three times respectively, and vacuum-dry at room temperature for 12 hours to obtain a solid upconversion fluorescent material, and its X-ray diffraction spectrum (XRD) and transmission electron microscope (TEM) are as follows: figure 2 shown; figu...

Embodiment 3

[0040] Take 2ml of rare earth nitrate solution (the mass of rare earth nitrate is 0.1458g, and the molar ratio of each rare earth ion is yttrium ion:ytterbium ion:erbium ion=80:18:2), add 18ml of absolute ethanol to it, and then add 0.3400 8ml of aqueous solution of polyethyleneimine (the mass ratio of rare earth nitrate to polyethyleneimine is 0.429:1), stirred for 10min; then add 0.1260g of sodium fluoride (F - / Ln 3+ Molar ratio of 6:1) aqueous solution 8ml, after stirring for 20min, put it in the autoclave, under the condition of stirring, hydrothermal reaction at 240℃ for 10h; stop heating and keep stirring to cool to room temperature, centrifuge to separate the solid product, use Wash each with absolute ethanol and ultrapure water 3 times, and vacuum-dry at room temperature for 12 hours to obtain a solid up-conversion fluorescent material. Its X-ray diffraction pattern (XRD) and transmission electron microscope pattern (TEM) are as follows: image 3 shown; image 3 The...

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Abstract

The invention discloses a preparation method of a water-soluble upconversion fluorescence nano material. The preparation method comprises the steps of (1) preparing a rare earth nitrate solution, wherein the molar ratio of yttrium irons to ytterbium ions to erbium ions in rare earth ions is (60-90):(5-35):(0.5-10); (2) adding lower alcohol and a water-soluble rare earth ion ligand and uniformly mixing, and adding a sodium fluoride aqueous solution to obtain mixed liquid, wherein in the mixed liquid, the molar ratio of fluorine ions to the total rare earth ions is (5-16):1, and the volume of fatty alcohol accounts for 1 / 3-1 / 2 of the volume of the mixed liquid; (3) performing a hydrothermal reaction on the obtained mixed liquid at 200-240 DEG C for 10-24 hours, and after the reaction, performing centrifugal separation on a solid product to obtain the upconversion fluorescence nano material. By adopting the preparation method disclosed by the invention, the prepared upconversion fluorescence nano material takes a hexagonal crystal phase as a main body, has relatively high upconversion luminous intensity and good water solubility, and is applicable to biological markers.

Description

technical field [0001] The invention belongs to the field of preparation of nano fluorescent materials, in particular to a preparation method of water-soluble up-conversion fluorescent nano materials. Background technique [0002] Up-conversion fluorescent nanomaterials are fluorescent nanomaterials that are excited by near-infrared and emitted by visible light. They have the advantages of large tissue penetration depth, no photodamage to living organisms, avoidance of biological body fluorescence, anti-photobleaching, safety and non-toxicity, etc. It has attracted more and more attention as a biomarker fluorescent material. The prerequisites for the application of upconversion fluorescent nanomaterials in biological analysis are high upconversion luminescence intensity, controllable size and morphology, good water solubility and coupling with biomolecules. [0003] The crystal phases of up-conversion fluorescent nanomaterials mainly include cubic crystal phase and hexagona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C30B29/60B82Y40/00B82Y20/00
Inventor 刘志洪杨利何梦媛吴正俊汤志恺王宇辉
Owner GUANGZHOU IMPROVE MEDICAL TECH CO LTD
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