Rare earth-doped NaGdF4 upconversion nanocrystalline and preparation method thereof

A rare earth doping, nanocrystalline technology, applied in nanotechnology, nano-optics, nanotechnology and other directions, can solve the problems of high reaction cost, unfavorable environmental protection, strong corrosion, etc., and achieve high phase purity, uniform size and high affinity. Effect

Inactive Publication Date: 2016-05-25
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current preparation of such materials is mainly obtained by decomposing trifluoroacetate at high temperature with oleic acid (OA) as a stabilizer and ligand and octadecene (ODE) as a solvent. During the reaction process of this method, strong Corrosive and toxic substances, not conducive to environmental protection, and high reaction costs

Method used

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  • Rare earth-doped NaGdF4 upconversion nanocrystalline and preparation method thereof
  • Rare earth-doped NaGdF4 upconversion nanocrystalline and preparation method thereof
  • Rare earth-doped NaGdF4 upconversion nanocrystalline and preparation method thereof

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Effect test

Embodiment 1

[0031] A Rare Earth Doped β-NaGdF 4 A preparation method for an up-conversion nanocrystalline material, comprising the steps of:

[0032] (1) According to the mass ratio of Gd:Yb:Er=78:20:2, the total amount of rare earth oxides (Ln 2 o 3 ) powder, put it into a container, add a small amount of deionized water, raise the temperature under magnetic stirring, set it at 100-135°C, when the temperature rises to 80°C, add 1.5mL hydrochloric acid dropwise, after a few minutes, the solid dissolves completely and becomes transparent solution; add 0.12g sodium hydroxide (NaOH) solid and 1mL oleic acid (OA) in another container, and heat up to 100-180°C under the condition of blowing Ar gas, until all the sodium hydroxide solid is dissolved to obtain an oily liquid;

[0033] (2) The transparent solution described in step (1) was evaporated to dryness at 150° C. under magnetic stirring in a fume hood to obtain a solid, which was mixed with the oily liquid described in step (1) and then...

Embodiment 2

[0039] A Rare Earth Doped β-NaGdF 4 A preparation method for an up-conversion nanocrystalline material, comprising the steps of:

[0040] (1) Gd:Yb:Er=81.5:18:0.5 weighs the total amount of rare earth oxide (Ln 2 o 3 ) powder, the follow-up steps are the same as (1) in Example 1, and the solid is completely dissolved to obtain a transparent solution, and the transparent solution is evaporated to dryness at 160°C under magnetic stirring in a fume hood to obtain a solid; in this container, add 0.12g sodium hydroxide (NaOH ) solid and 1mL oleic acid (OA), the temperature was raised to 140° C. under the condition of feeding Ar gas, until all the solids were dissolved to obtain an oily liquid;

[0041] (2) Add 6ml of ethanol, 3.5ml of hexane, and 4ml of deionized aqueous solution to the oily liquid described in step (1), then leave to stand for stratification, get the upper layer liquid, wash three times with deionized water, discard the lotion, After washing, it was heated to 6...

Embodiment 3

[0045] A Rare Earth Doped β-NaGdF 4 A preparation method for an up-conversion nanocrystalline material, comprising the steps of:

[0046] (1) According to the mass ratio of Gd:Yb:Tm=78:20:2, the total amount of rare earth oxides (Ln 2 o 3 ) powder, subsequent steps are with step (1) in example 1;

[0047] (2) The transparent solution described in step (1) was evaporated to dryness at 150° C. under magnetic stirring in a fume hood to obtain a solid, which was mixed with the oily liquid described in step (1) and then added to 6ml of ethanol and 3.5ml of hexane , 4ml of deionized water solution, magnetically stirred at room temperature for 4 hours, the liquid was poured into a separatory funnel, separated, the upper liquid was washed three times with deionized water, discarded the lotion, stirred and heated to 80°C after washing, and a waxy solid was obtained , add a mixed solution of 8mL oleylamine and 8mL octadecene, heat up to 160°C while stirring under the protective gas A...

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Abstract

The invention belongs to the technical field of luminescent materials, and particularly relates to a rare earth-doped NaGdF4 upconversion nanocrystalline and a preparation method thereof. The chemical expression formula of the rare earth-doped NaGdF4 upconversion nanocrystalline is beta-NaGd(100-X-Y)F4:X%Yb<3+>, Y%Er<3+> or beta-NaGd(100-X-Y)F4:X%Yb<3+>, Y%Tm<3+>, the value range of X is 10-90, and the value range of Y is 0.5-3. According to the rare earth-doped NaGdF4 upconversion nanocrystalline and the preparation method thereof, the Yb<3+> and Er<3+>-doped or Yb<3+> and Tm<3+>-doped beta-NaGdF4 upconversion nanocrystalline material is prepared through a high-temperature thermal cracking method and a solvothermal method, the preparation technology is simple and easy to operate, and the preparation cost of a multicolor luminescent material is greatly lowered; in addition, the preparation process is green and environmentally friendly, and the potential application value in the fields of solid lasers, solar cells, infrared radiation detection, biomedical imaging and the like is achieved.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, in particular to a rare earth doped NaGdF 4 Up-conversion nanocrystals and methods for their preparation. Background technique [0002] In recent years, due to the potential application value of up-conversion in solid-state lasers, three-dimensional displays, solar cells, photocatalysis, biomarkers, and photodynamic therapy, it has attracted much attention, especially the rare earth-doped fluoride ALnF 4 (A = alkali metal or alkaline earth metal, Ln = rare earth element) up-conversion materials have been extensively studied in recent years. β-NaYF 4 It has been recognized as one of the matrix materials with the strongest luminous efficiency. In recent years, β-(K-Na)GdF has been discovered 4 Matrix can not only provide NaYF-like 4 Up-conversion luminescence, and multimodal imaging, such as CT and MRI, can replace traditional toxic enhancers. due to Gd 3+ With abundant energy l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85B82Y30/00B82Y20/00
CPCB82Y20/00B82Y30/00C09K11/7773
Inventor 王友法赵书文王颖周斌
Owner WUHAN UNIV OF TECH
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