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Preparation method for carboxyl functionalized beta-NaYF4 substrate upconversion fluorescence nanomaterial

A technology of fluorescent nanomaterials and carboxyl functionalization, which is applied in the field of preparation of up-conversion fluorescent materials, can solve the problems of complicated and tedious operation steps, incapable of large-scale production, high labor intensity, etc., and achieves simple and safe operation, few kinds of raw materials, and water solubility. good effect

Inactive Publication Date: 2012-10-24
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a carboxyl functionalized β-NaYF 4 Fabrication method of matrix upconversion fluorescent nanomaterials to address carboxyl-functionalized β-NaYF 4 There are many kinds of raw materials for the preparation of up-conversion fluorescent nanomaterials, the operation steps are complicated and cumbersome, the preparation is labor-intensive, and the problem of inability to scale production

Method used

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  • Preparation method for carboxyl functionalized beta-NaYF4 substrate upconversion fluorescence nanomaterial
  • Preparation method for carboxyl functionalized beta-NaYF4 substrate upconversion fluorescence nanomaterial
  • Preparation method for carboxyl functionalized beta-NaYF4 substrate upconversion fluorescence nanomaterial

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Accurately weigh 5 mmol of NH in a beaker 4 F solid, add 15 mL ethylene glycol solvent, sonicate for about 20 min to make NH 4 The F solid is completely dissolved to obtain solution A;

[0032] (2) Accurately weigh a total of 1.2 mmol of rare earth chloride (RECl 3 ) (RE=Y, Yb, Er; Y:Yb:Er = 80:18:2), 0.4 g sodium polyacrylate, the molecular weight of sodium polyacrylate is Mw = 5100, and 2.4 mmol sodium chloride, add 20 mL ethyl Diol, obtain solution B after ultrasonic dispersion;

[0033] (3) First transfer the B solution to a 50 mL autoclave, then add A to B under rapid stirring, continue to stir for 10 min to make it evenly mixed, tightly cover the autoclave, and react at 200 °C 12 hours;

[0034] (4) After the reaction, the reactants in the reactor were centrifuged, washed twice with water, and dried at 60°C to obtain carboxyl-functionalized β-NaYF 4 : Yb, Er up-conversion nano-fluorescent materials.

[0035] The prepared carboxyl functionalized β-NaYF 4...

Embodiment 2

[0038] (1) Weigh 5 mmol of NH in a beaker 4 F solid, add 15 mL ethylene glycol solvent, sonicate for about 20 min to make NH 4 F is completely dissolved to obtain solution A;

[0039](2) Accurately weigh a total of 1.2 mmol of rare earth chloride (RECl 3 ) (RE=Y,Yb,Tm; Y:Yb:Tm = 78:20:2), 0.4 g sodium polyacrylate, the molecular weight of sodium polyacrylate is Mw = 5100, and 2.4 mmol NaCl, add 20 mL ethylene glycol , solution B was obtained after ultrasonic dispersion;

[0040] (3) First transfer the B solution to a 50 mL autoclave, then add A to B under rapid stirring, continue to stir for 10 min to make it evenly mixed, tightly cover the autoclave, and react at 200 °C 12 hours;

[0041] (4) After the reaction, the product in the reactor was centrifuged, washed twice with water, and dried at 60°C to obtain carboxyl-functionalized β-NaYF 4 : Yb, Tm up-conversion nano-fluorescent material.

[0042] The prepared carboxyl functionalized β-NaYF 4 The fluorescence spectrum ...

Embodiment 3

[0044] (1) Weigh 5 mmol of NH in a beaker 4 F solid, add 15 mL ethylene glycol solvent, sonicate NH 4 F is completely dissolved to obtain solution A;

[0045] (2) Accurately weigh a total of 1.2 mmol of rare earth chloride (RECl 3 ) (RE=Y,Yb,Er; Y:Yb:Er = 80:18:2) and 0.4 g sodium polyacrylate, the molecular weight of sodium polyacrylate is Mw = 5100, add 20 mL ethylene glycol, and obtain after ultrasonic dispersion Solution B;

[0046] (3) First transfer the B solution to a 50 mL autoclave, then add A to B under rapid stirring, continue to stir for 10 min to make it evenly mixed, tightly cover the autoclave, and react at 200 °C 12 hours;

[0047] (4) After the reaction, the product in the reactor was centrifuged, washed twice with water, and dried at 60°C to obtain carboxyl-functionalized β-NaYF 4 : Yb, Er up-conversion nano-fluorescent materials.

[0048] The prepared carboxyl functionalized β-NaYF 4 The transmission electron microscope image of the matrix up-conversi...

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Abstract

The present invention discloses a preparation method for a carboxyl functionalized beta-NaYF4 substrate upconversion fluorescence nanomaterial. The method comprises the following steps: (a) dissolving 5-15 mmol of ammonium fluoride solid in a solvent to obtain a solution A; (b) weighing a rare earth salt mixture with a total amount of 1.2 mmol, 0.3-1.0 g of sodium polyacrylate, and 0-9.6 mmol of sodium chloride, and adding the materials to a solvent to obtain a solution B; (c) sequentially transferring the solution B and the solution A to a high pressure reactor, rapidly stirring for uniform mixing, and carrying out a reaction for 12-36 hours at a temperature of 180-220 DEG C; and (d) taking the reaction product out of the high pressure reactor, and carrying out centrifugation, separation, washing and drying on the reaction product. The method of the present invention has the following advantages that: the variety of the required materials is less, the operation is simple, the method is applicable for large scale production, and the prepared product surface is rich in carboxylate, wherein the carboxylate is easily linked with proteins and other biological macromolecules, such thatthe product can be widely used in fields of biomarkers and clinical detection.

Description

technical field [0001] The present invention relates to the preparation method of up-conversion fluorescent material, specifically a kind of β-NaYF that uses sodium polyacrylate as ligand to prepare carboxyl functionalization 4 Methods for Upconversion of Fluorescent Nanomaterials on Substrates. Background technique [0002] β-NaYF 4 It is one of the up-conversion fluorescent matrix materials with the highest luminous efficiency known at present, and it has excellent application effects in the fields of biomarkers and medical clinical detection. But β-NaYF 4 Up-conversion fluorescent nanomaterials are easily affected by organic ligands such as oleic acid, oleylamine or linoleic acid in the current preparation methods, and the prepared products are often not easily soluble in water and have poor biocompatibility. For the field of biomarkers or medical clinical testing, they require β-NaYF 4 Must have good water solubility and biocompatibility, so technicians are preparing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/02C12Q1/02
Inventor 刘成辉李正平王哲
Owner HEBEI UNIVERSITY
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