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Porous rare earth doped Li4ZrF8 up-conversion nano crystal and preparation method thereof

A rare earth doping, nanocrystalline technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of complex process and reduced luminous efficiency, and achieve the effect of huge development potential, excellent luminescence performance, and strong up-conversion luminescence ability.

Inactive Publication Date: 2018-08-03
HUZHOU TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process of this scheme is complicated, and the overall luminous efficiency of the up-conversion material will be significantly reduced after being coated with a layer of porous silicon dioxide.

Method used

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  • Porous rare earth doped Li4ZrF8 up-conversion nano crystal and preparation method thereof
  • Porous rare earth doped Li4ZrF8 up-conversion nano crystal and preparation method thereof
  • Porous rare earth doped Li4ZrF8 up-conversion nano crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1, Li 4 ZrF 8 : 18mol% Yb 3+ , 2mol% Er 3+ preparation of

[0036]At room temperature, measure 1.7mL zirconium acetate, weigh 0.0825g ytterbium acetate and 0.0090g erbium acetate, add 0.0958g lithium hydroxide to a 100mL three-necked flask, add 8mL oleic acid and 12mL octadecene, stir to mix evenly. The three-necked flask was evacuated, and then nitrogen gas was introduced. In a nitrogen atmosphere, the above mixture was heated to 120°C and kept at this temperature for 30 minutes to completely dissolve the zirconium acetate and rare earth acetate to obtain a clear solution, which was then cooled to room temperature. Weigh 0.2963g of ammonium fluoride and dissolve it in 6mL of methanol solution, stir and react at room temperature for 30 minutes. Then the mixed solution was heated to 60° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was removed, it was heated to 280°C in a nitrogen atmosphere, kept for 40 minutes, t...

Embodiment 2

[0040] Example 2, Li 4 ZrF 8 : 18mol% Yb 3+ , 2mol% Er 3+ preparation of

[0041] Measure 1.7mL of zirconium acetate at room temperature, weigh 0.0825g of ytterbium acetate and 0.0090g of erbium acetate, add 0.0958g of lithium hydroxide into a 100mL three-necked flask, add 8mL of oleic acid and 12mL of octadecene, and stir to mix evenly. The three-necked flask was evacuated, and then nitrogen gas was introduced. In a nitrogen atmosphere, the above mixture was heated to 120°C and kept at this temperature for 30 minutes to completely dissolve the zirconium acetate and rare earth acetate to obtain a clear solution, which was then cooled to room temperature. Weigh 0.2668g of ammonium fluoride and dissolve it in 6mL of methanol solution, stir and react at room temperature for 30 minutes. Then the mixed solution was heated to 60° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was removed, it was heated to 280°C in a nitrogen atmosphere...

Embodiment 3

[0042] Example 3, Li 4 ZrF 8 : 18mol% Yb 3+ , 2mol%Tm 3+ preparation of

[0043] Measure 1.7mL of zirconium acetate at room temperature, weigh 0.0825g of ytterbium acetate and 0.0091g ​​of thulium acetate, add 0.0958g of lithium hydroxide into a 100mL three-neck flask, add 8mL of oleic acid and 12mL of octadecene, and stir to mix evenly. The three-necked flask was evacuated, and then nitrogen gas was introduced. In a nitrogen atmosphere, the above mixture was heated to 120°C and kept at this temperature for 30 minutes to completely dissolve the zirconium acetate and rare earth acetate to obtain a clear solution, which was then cooled to room temperature. Weigh 0.2668g of ammonium fluoride and dissolve it in 6mL of methanol solution, stir and react at room temperature for 30 minutes. Then the mixed solution was heated to 60° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was removed, it was heated to 280°C in a nitrogen atmosphere...

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Abstract

The invention discloses a porous rare earth doped Li4ZrF8 up-conversion nano crystal and a preparation method thereof. The up-conversion nano crystal is the monoclinic phase Li4ZrF8 nano crystal, thesize of the Li4ZrF8 nano crystal is 20-60 nanometers, and the nano crystal has a lot of micropores. The preparation method comprises the following steps: 1) dissolving lithium hydroxide, rare earth acetate and zirconium acetate in a solvent; 2) adding an alcoholic solution dissolved with ammonium fluoride in the solution obtained in the step 1), and heating the material to remove alcohol; and 3) heating the solution after alcohol is removed, cooling the material to room temperature, and preparing the rare earth doped Li4ZrF8 up-conversion nano crystal. The preparation method has the advantagesof simple process and good repeatability, and a prepared nano luminescent material has the advantages of dispersibility and good homogeneity. The prepared Li4ZrF8 nano crystal has strong up-conversion luminescence capability, has medicine slow-release capability, and has large application prospect on the fields of bioluminescence imaging and tumour drug treatment.

Description

technical field [0001] The invention belongs to the field of manufacturing nano-luminescent materials, and relates to an up-conversion nano-luminescent material, in particular to porous rare earth-doped Li 4 ZrF 8 Up-conversion nanocrystals and methods for their preparation. Background technique [0002] Rare-earth-doped upconversion nanocrystals have the advantages of deep tissue penetration and small tissue background fluorescence interference, and have important application prospects in the fields of bioluminescent labeling and immunoassay, and thus have attracted widespread attention from scholars at home and abroad. Among the host materials of upconversion nanocrystals, fluoride has the advantages of low phonon energy, good physical and chemical stability, and low toxicity. It is a kind of host material of upconversion nanocrystals with excellent performance. The most studied fluoride nanocrystals are rare earth fluoride nanocrystals, while the research on rare earth ...

Claims

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Application Information

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IPC IPC(8): C09K11/67
CPCC09K11/7773
Inventor 罗文钦巫海燕李彬周宁陈锦
Owner HUZHOU TEACHERS COLLEGE
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