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Rare earth-doped alkaline earth metal fluoride nano material, and preparation method and application thereof

An alkaline earth metal and rare earth doping technology, which is applied in the direction of luminescent materials, material excitation analysis, chemical instruments and methods, etc., can solve the problems of core-shell structure growth, long reaction time, energy consumption, etc., and achieve simple operation and uniform particle size Controllable and repeatable effect

Active Publication Date: 2013-07-31
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvothermal method requires a special reaction device (autoclave), and the reaction time is longer (12-36 hours), which consumes more energy; in addition, the solvothermal method cannot grow the core-shell structure, which is very important for the upconversion luminescence of small nanoparticles. Very unfavorable, often the smaller the particle, the more severe the upconversion luminescence quenching of rare earth ions by the groups on the surface, and coating a shell on the basis of the original core is a good solution to improve the upconversion luminescence, but Solvothermal methods cannot do this yet

Method used

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  • Rare earth-doped alkaline earth metal fluoride nano material, and preparation method and application thereof
  • Rare earth-doped alkaline earth metal fluoride nano material, and preparation method and application thereof
  • Rare earth-doped alkaline earth metal fluoride nano material, and preparation method and application thereof

Examples

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Effect test

example 1

[0056] Example 1: CaF 2 : Preparation of 5%Eu, 5%Na nanomaterials.

[0057] Weigh 0.167 g Ca(CH 3 COO) 2 ·H 2 O with 0.02g Eu(CH 3 COO) 3 4H 2 O, then add 5 mL of oleic acid and 15 mL of octadecene, heat to 160 °C with nitrogen gas and keep it warm for 30 minutes to form a transparent solution A, then cool down to room temperature; another 0.084 g of NH 4 Dissolve F and 0.084 g NaOH in 10 mL of methanol to form a transparent solution B, add solution B to solution A to form a mixed solution C, then heat to 60 °C and keep it warm for 30 minutes to remove methanol, heat up to 280 °C and keep it warm for 1 hour Cool down to room temperature, add 30 mL of acetone to precipitate, separate and wash to obtain oil-soluble CaF with an average size of 4 nm 2 : 5%Eu, 5%Na nanoparticles. Disperse the oil-soluble nanoparticles in 10 mL of cyclohexane, add 10 mL of dichloromethane solution dissolved with 30 mg of nitrous tetrafluoroborate, mix and react for 30 minutes, then centrifug...

example 2

[0058] Example 2: CaF 2 : Preparation of 5%Ce, 5%Tb, 10%Na nanomaterials. With 0.158 g Ca(CH 3 COO) 2 ·H 2 O, 0.02g Ce(CH 3 COO) 3 4H 2 O and 0.02g Tb(CH 3 COO) 3 4H 2 O is a raw material, and the synthesis steps are as in Example 1, and the water-soluble CaF with an average size of 4nm is finally obtained. 2 : 5%Ce, 5%Tb, 10%Na nanomaterials.

example 3

[0059] Example 3: CaF 2 : Preparation of 0.5%Er, 18%Yb, 18%Na nanoparticles. With 0.144 g Ca(CH 3 COO) 2 ·H 2 O, 0.002g Er(CH 3 COO) 3 4H 2 O and 0.076g Yb(CH 3 COO) 3 4H 2 O is a raw material, and the synthesis steps are as in Example 1, and the water-soluble CaF with an average size of 4nm is finally obtained. 2 : 0.5%Er, 18%Yb, 18%Na nanomaterials.

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Abstract

The invention discloses a water-soluble rare earth-doped alkaline earth metal fluoride nano material with the following components: xLn<3+>-yNa<+>-[1-(x+y)]MF2, wherein Ln<3+> is selected one or any number from Ce<3+>, Yb<3+>, Er<3+>, Tm<3+>, Ho<3+>, Eu<3+>, Gd<3+>, Tb<3+>, Dy<3+>, Sm<3+>, Nd<3+> or Pr<3+>; M is selected from Ca, Sr or Ba; x is larger than 0 mol% and smaller than or equal to 50 mol%; and y is larger than 0 mol%and smaller than or equal to 50 mol%. The material has relatively good water solubility and luminescent performance, and can be applied in the fields such as biological detection, biological imaging, etc.

Description

technical field [0001] The invention relates to a rare-earth-doped inorganic nanometer material and its preparation and application, in particular to the synthesis of a water-soluble rare-earth-doped alkaline-earth metal fluoride nanometer fluorescent labeling material and its application in the fields of fluorescent biological detection and biological imaging. Background technique [0002] In recent years, rare-earth-doped phosphors have received widespread attention. These materials have shown great application value in some traditional fields such as mercury-free fluorescent lamps, flat panel displays, solid-state lasers, optical storage, LEDs, and solar cells. What attracts people's attention is the application of rare earth-doped inorganic nanomaterials in fluorescent biomarkers. Compared with traditional fluorescent labeling materials (such as fluorescent dyes and quantum dots), rare earth-doped inorganic nanomaterials have high chemical stability, long fluorescence li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61G01N21/64A61K49/00
Inventor 陈学元郑伟涂大涛刘永升朱浩淼
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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