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A preparation method and application of rare earth-doped apatite fluorescent nanodots

A fluorescent nano and rare earth doping technology, applied in nanotechnology, nano optics, nanotechnology, etc., can solve the problems of nanoparticle agglomeration, size increase, and impact on the use of fluorescent imaging agents, and achieve reduced agglomeration, uniform size distribution, and good Effects of Aqueous Suspension Stability and Fluorescence Properties

Active Publication Date: 2020-08-04
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the heat treatment process often leads to problems such as agglomeration and size increase of nanoparticles, which affect their use as fluorescent imaging agents.

Method used

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  • A preparation method and application of rare earth-doped apatite fluorescent nanodots
  • A preparation method and application of rare earth-doped apatite fluorescent nanodots
  • A preparation method and application of rare earth-doped apatite fluorescent nanodots

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Prepare 15ml of colloidal solution of polyacrylic acid, calcium ions, and rare earth ions, adjust the pH to 9.0 with ammonia water, and stir for 15 minutes. Among them, Eu 3+ / (Ca 2+ +Eu 3+ ) The mole fraction is 4%. Mix 15ml of phosphate ion solution with the obtained colloidal solution, adjust the pH to 9.7 with ammonia water and stir vigorously for 30min to obtain a milky white suspension. Among them, (Ca 2+ +Eu 3+ ) / P mole fraction is 1.67, carboxylate and (Ca 2+ +Eu 3+ ) The molar ratio is 0.92, (Ca 2+ +Eu 3+ ), PO 4 3- and PAA concentrations were 0.0501M, 0.03M and 4mg / ml, respectively. The obtained milky white suspension was hydrothermally treated at 60° C. for 1 h (the average temperature increase rate was 12° C. / min), centrifuged and washed to rare earth-doped apatite fluorescent nano-dots.

[0029] The rare earth-doped apatite fluorescent nano-dot transmission electron microscope picture and the particle size distribution histogram obtained in this...

Embodiment 2

[0031] Prepare 15ml of colloidal solution of polyacrylic acid, calcium ions, and rare earth ions, adjust the pH to 5.0 with ammonia water, and stir for 15 minutes. Among them, Eu 3+ / (Ca 2+ +Eu 3+ ) The mole fraction is 4%. Mix 15ml of phosphate ion solution with the obtained colloidal solution, adjust the pH to 9.7 with ammonia water and stir vigorously for 30min to obtain a milky white suspension. Among them, (Ca 2+ +Eu 3+ ) / P mole fraction is 1.67, carboxylate and (Ca 2+ +Eu 3+ ) The molar ratio is 0.92, (Ca 2+ +Eu 3+ ), PO 4 3- and PAA concentrations were 0.0501M, 0.03M and 4mg / ml, respectively. The obtained milky white suspension was transferred into an autoclave, and subjected to hydrothermal treatment at 180° C. for 1 h (the average temperature increase rate was 5.1° C. / min) to obtain a suspension of rare earth-doped apatite fluorescent nanodots. After centrifugation and washing, the rare earth-doped apatite fluorescent nano-dots are obtained.

[0032] The ...

Embodiment 3

[0034] Prepare 15ml of colloidal solution of polyacrylic acid, calcium ions, and rare earth ions, adjust the pH to 9.0 with ammonia water, and stir for 15 minutes. Among them, Eu 3+ / (Ca 2+ +Eu 3+ ) The mole fraction is 4%. Mix 15ml of phosphate ion solution with the obtained colloidal solution, adjust the pH to 9.7 with ammonia water and stir vigorously for 30min to obtain a milky white suspension. Among them, (Ca 2+ +Eu 3+) / P mole fraction is 1.67, carboxylate and (Ca 2+ +Eu 3+ ) The molar ratio is 0.46, (Ca 2+ +Eu 3+ ), PO 4 3- and PAA concentrations were 0.0501M, 0.03M and 2mg / ml, respectively. The obtained milky white suspension was transferred into an autoclave, hydrothermally treated at 120° C. for 1 h (the average heating rate was 10° C. / min), centrifuged and washed to obtain rare earth-doped apatite fluorescent nanodots.

[0035] The rare earth-doped apatite fluorescent nano-dot transmission electron microscope picture and the particle size distribution hi...

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Abstract

The invention discloses a preparation method for rare-earth doped apatite fluorescence nano points and application. The preparation method comprises the following steps: firstly, preparing a colloidalsolution with polyacrylic acid, calcium ions and rare-earth ions, and adjusting the pH value of the colloidal solution to 4-9 by using ammonium hydroxide; secondly, mixing the colloidal solution witha phosphate anion solution according to a ratio, and adjusting the pH value to 9-10 by using ammonium hydroxide to obtain a milk white suspension; finally heating to perform hydrothermal treatment onthe suspension, centrifuging, and washing, thereby obtaining the rare-earth doped apatite fluorescence nano points. By adopting the preparation method, controllable preparation of the rare-earth doped apatite fluorescence nano points is achieved, the size of the nano points is controlled within 2.0-10nm, and the rare-earth doped apatite fluorescence nano points have good water suspension stability and fluorescence properties and can be used as a biological imaging agent which is applied to in-vivo / in-vitro fluorescence imaging.

Description

technical field [0001] The invention relates to the technical field of preparation of nano-dot materials, in particular to a method for preparing rare earth-doped apatite fluorescent nano-dots and the application of the fluorescent nano-dot material in the field of in vivo and in vitro fluorescence imaging. Background technique [0002] Early diagnosis of cancer is the key to effective treatment, and fluorescent nanoparticles can realize the labeling and early diagnosis of tumor cells. Fluorescent nanoparticles mainly include: polymer fluorescent nanoparticles, semiconductor quantum dots, and lanthanide-doped nanoparticles. The first two nanoparticles have shortcomings such as low optical stability and toxicity, which hinder their application in vivo and in vitro fluorescence imaging. Lanthanide-doped nanoparticles have been developed into new nanoparticles that can replace polymer fluorescent nanoparticles and semiconductor quantum dots, which are characterized by Stokes sh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/81A61K49/00G01N21/64B82Y20/00B82Y40/00
Inventor 韩颖超邢庆国何王美戴红莲
Owner WUHAN UNIV OF TECH
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