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Preparation method of ultra-small nayf4: Yb3+, Er3+ upconversion luminescent material

A technology of luminescent materials and nanoparticles, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of large size of luminescent materials, and achieve the effect of small size, uniform particle size distribution, and no impurity phase

Inactive Publication Date: 2015-09-09
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Technical problem: the present invention is aimed at the current NaYF 4 :Yb 3+ ,Er 3+ The problem of large size of up-conversion luminescent materials, providing an ultra-small NaYF 4 :Yb 3+ ,Er 3+ Preparation method of up-conversion nanoparticle luminescent material

Method used

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  • Preparation method of ultra-small nayf4: Yb3+, Er3+ upconversion luminescent material
  • Preparation method of ultra-small nayf4: Yb3+, Er3+ upconversion luminescent material
  • Preparation method of ultra-small nayf4: Yb3+, Er3+ upconversion luminescent material

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Experimental program
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Embodiment 1

[0024] (1) Dissolve 1.0mmol rare earth acetate in 6ml OA and 15ml ODE, Y:Yb:Er=78:20:2 in the rare earth acetate, heat to 100~130℃ and stir for 30~40min to form a uniform (2) When the temperature drops to 50-60°C, the NH dissolved in methanol 4 F was added to the solution together with NaOH and stirred for 30-40min, in which NH 4 F and NaOH are 4mmol and 2.5mmol respectively; (3) After removing methanol, the temperature of the solution is raised to 300°C for 90min, and then cooled to room temperature to obtain NaYF 4 :Yb 3+ ,Er 3+ Up-converting nanoparticles; (4) Washing the prepared up-converting nanoparticles with ethanol three times and then dispersing them in n-hexane.

[0025] The sample is a pure hexagonal phase structure with a size of about 24.6nm, such as figure 1 shown.

Embodiment 2

[0027] (1) Dissolve 0.5mmol rare earth acetate in 6ml OA and 15ml ODE, Y:Yb:Er=78:20:2 in the rare earth acetate, heat to 100~130℃ and stir for 30~40min to form a uniform (2) When the temperature drops to 50-60°C, the NH dissolved in methanol 4 F was added to the solution together with NaOH and stirred for 30-40min, in which NH 4 F and NaOH are 2mmol and 1.25mmol respectively; (3) After removing methanol, the temperature of the solution is raised to 300°C for 90min, and then cooled to room temperature to obtain NaYF 4 :Yb 3+ ,Er 3+ Up-converting nanoparticles; (4) Washing the prepared up-converting nanoparticles with ethanol three times and then dispersing them in n-hexane.

[0028] The sample is a pure hexagonal phase structure with a size of about 18.2nm, such as figure 2 shown.

Embodiment 3

[0030] (1) Dissolve 0.3mmol rare earth acetate in 30ml OA and 100ml ODE, Y:Yb:Er=78:20:2 in the rare earth acetate, heat to 100~130℃ and stir for 30~40min to form a uniform (2) When the temperature drops to 50-60°C, the NH dissolved in methanol 4 F was added to the solution together with NaOH and stirred for 30-40min, in which NH 4 F and NaOH are 1.2mmol and 0.75mmol respectively; (3) After removing methanol, raise the solution temperature to 300°C for 90min, then cool to room temperature to obtain NaYF 4 :Yb 3+ ,Er 3+ Up-conversion nanoparticles; (4) Wash the prepared up-conversion nanoparticles with ethanol three times and then disperse them in n-hexane.

[0031] The sample is a pure hexagonal phase structure with a size of about 17.7nm, such as image 3 shown.

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Abstract

The invention provides a preparation method of an ultrasmall NaYF4:Yb<3+>,Er<3+> upconversion nanoparticle luminescent material, which comprises the following steps: a) lowering the upconversion nanoparticle size by lowering the rare earth acetate concentration in the reactants or regulating the contents of oleic acid and 1-octadecene; and b) controlling the nucleating and crystallizing process by the repeated oscillation design of reaction temperature, thereby further lowering the upconversion nanoparticle size. The ultrasmall NaYF4:Yb<3+>,Er<3+> upconversion nanoparticles prepared by the method have the advantages of small size (9-18nm), uniform particle size distribution and high luminescence efficiency, and are a hexagonal phase; and the preparation method has very high repeatability and favorable application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of rare earth up-conversion luminescent nanomaterials, in particular to an ultra-small NaYF 4 :Yb 3+ ,Er 3+ Preparation method of up-conversion luminescent material. Background technique [0002] An up-conversion luminescent material is a luminescent material that can convert near-infrared light into visible light. Utilizing this anti-Stokes effect, up-conversion luminescent materials have broad application prospects in many research fields, such as solid-state lasers, laser anti-counterfeiting, three-dimensional display, and biomedicine. Especially when used as a fluorescent labeling material, since its excitation light is 980nm near-infrared light, which is just in the light transmission window (630-1350nm) of biological tissue, it can not only effectively avoid the damage of short-wave excitation source to biological tissue, but also can Improve the detection depth of biological tissue, reduce it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85
Inventor 李东东邵起越蒋建清董岩方峰
Owner SOUTHEAST UNIV
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