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Preparation method of water-soluble upconversion fluorescent nano material

A fluorescent nanomaterial and water-soluble technology, which is applied in the direction of luminescent materials, nanotechnology, chemical instruments and methods, etc., can solve the problems affecting the application of biomarker materials, low up-conversion luminous intensity, and complicated pretreatment operations, etc., to achieve suitable Suitable for mass production, safe and non-toxic reaction process, good water solubility

Active Publication Date: 2014-02-19
GUANGZHOU IMPROVE MEDICAL TECH CO LTD
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  • 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 fluorescent nano material
  • Preparation method of water-soluble upconversion fluorescent nano material
  • Preparation method of water-soluble upconversion fluorescent nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 2ml of rare earth nitrate solution (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 0.9000g polyacrylic acid (polyacrylic acid and total Rare earth ion molar ratio is 1:1) aqueous solution 14ml, stir for 10min; then add 0.2100g sodium fluoride (fluoride ion to total rare earth ion molar ratio is 10:1) aqueous solution 8ml, after stirring for 20min, place in In a high-pressure reactor, react at 200 ° C for 10 h under stirring conditions; stop heating and keep stirring to cool to room temperature, centrifuge to separate the solid product, wash 3 times with absolute ethanol and ultrapure water, and vacuum dry at room temperature for 12 h to obtain a solid Up-conversion fluorescent material, its X-ray diffraction spectrum (XRD) and transmission electron microscope (TEM) are as follows figure 1 shown; figure 1 The X-ray diffraction pattern of A shows that the material is a mixed c...

Embodiment 2

[0037] Take 2 ml of rare earth nitrate solution (the molar ratio of each rare earth ion is yttrium ion: ytterbium ion: erbium ion = 80:18:2), add 18 ml of absolute ethanol to it, and then add 0.9000 g of polyacrylic acid (polyacrylic acid and total 8ml of an aqueous solution containing 0.2100g of sodium fluoride (the molar ratio of fluoride ions to total rare earth ions is 10:1) was added, stirred for 10min, stirred for 20min, and placed in In a high-pressure reactor, react at 200 ° C for 10 h under stirring conditions; stop heating and keep stirring to cool to room temperature, centrifuge to separate the solid product, wash 3 times with absolute ethanol and ultrapure water, and vacuum dry at room temperature for 12 h to obtain a solid Up-conversion fluorescent material, its X-ray diffraction spectrum (XRD) and transmission electron microscope (TEM) are as follows figure 2 shown; figure 2 The X-ray diffraction pattern of A shows that the material is a mixed crystal phase of...

Embodiment 3

[0039] Take 2 ml of rare earth nitrate solution (the molar ratio of each rare earth ion is yttrium ion: ytterbium ion: erbium ion = 80:18:2), add 18 ml of absolute ethanol to it, and then add 0.340 g of polyethyleneimine (polyethyleneimine Add 8ml of an aqueous solution containing 0.2100g of sodium fluoride (the molar ratio of fluoride ions to total rare earth ions is 10:1) and stir for 10 minutes. After 20 minutes, put it in a high-pressure reactor, and conduct a hydrothermal reaction at 240°C for 10 hours under stirring; stop heating and keep stirring to cool to room temperature, centrifuge to separate the solid product, wash 3 times with absolute ethanol and ultrapure water, Vacuum drying at room temperature for 12 hours to obtain a solid up-conversion fluorescent material, its X-ray diffraction spectrum (XRD) and transmission electron microscope (TEM) as image 3 shown; image 3 The X-ray diffraction spectrum of A shows that the material is a pure hexagonal crystal phase;...

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Abstract

The invention discloses a preparation method of a water-soluble upconversion fluorescent nano material. The preparation method comprises following steps: a rare earth nitrate solution containing yttrium ions, ytterbium ions and erbium ions is prepared, a fatty alcohol and a water-soluble rare earth ion ligand are added for uniform mixing, and sodium fluoride aqueous solution is added so as to obtain a mixed solution, wherein (1) molar ratio of fluorinion to the total rare earth ion is (5-16):1, and (2) volume ratio of the fatty alcohol to water in the mixed solution is (0.5-1):1; the mixed solution is subjected to hydrothermal reaction at a temperature of 200 to 240 DEG C, is cooled to room temperature, and is subjected to centrifugation to separate a solid product, and then the water-soluble upconversion fluorescent nano material is obtained. The water-soluble upconversion fluorescent nano material is mainly of hexagonal phase, up-conversion luminescent intensity is high, water solubility is relatively high, and the water-soluble upconversion fluorescent nano material is suitable to be used as a biological marker.

Description

technical field [0001] The invention relates to a preparation method of an up-conversion fluorescent nanometer material, in particular to a preparation method of a water-soluble upconversion fluorescent nanometer material with high upconversion luminous intensity. 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 fluoresce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06B82Y40/00
Inventor 刘志洪杨利何梦媛孙靖王宇辉
Owner GUANGZHOU IMPROVE MEDICAL TECH CO LTD
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