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Method for preparing rare earth doped beta-NaYF4 upconversion nanocrystal with size of less than 8nm

A rare earth doping, nanocrystalline technology, applied in nanotechnology, nanooptics, nanotechnology, etc., to achieve high repeatability and promote transformation.

Active Publication Date: 2017-07-18
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the synthesis of small size (less than 10nm) β-NaYF 4 None of the nanocrystalline methods can effectively avoid the α-NaYF 4 Formation of heterogeneous phase

Method used

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  • Method for preparing rare earth doped beta-NaYF4 upconversion nanocrystal with size of less than 8nm
  • Method for preparing rare earth doped beta-NaYF4 upconversion nanocrystal with size of less than 8nm
  • Method for preparing rare earth doped beta-NaYF4 upconversion nanocrystal with size of less than 8nm

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) First, weigh 1mmol RECl of rare earth 3 ·6H 2 O (Y:Yb:Er=80:18:2, molar ratio) was added to 6 mL of oleic acid and 15 mL of l-octadecene solution. Under the protection of argon, stir and heat to 150°C and keep it warm for 30min. After the rare earth particles are completely dissolved, cool naturally to room temperature.

[0027](2) Then, successively dissolve 2.5mmol sodium oleate and 4mmol NH 4 10 mL methanol solution of F was added dropwise to the reaction system, stirred and heated to 60°C and kept for 60 min.

[0028] (3) Subsequently, under the protection of argon, the solution was stirred and heated to 300°C, kept for 0 min, and then naturally cooled to room temperature.

[0029] (4) Centrifuge with a centrifuge, wash and centrifuge repeatedly with cyclohexane-ethanol three times, and finally disperse in cyclohexane or dry in an oven.

[0030] (5) Under the experimental conditions, uniformly dispersed pure phase β-NaYF with a size of 7.0 nm can be obtained...

Embodiment 2

[0032] (1) First, weigh 1mmol RE(Ac) of rare earth 3 ·nH 2 O (Y:Yb:Tm=78:18:4, molar ratio) was added to 6 mL of oleic acid and 15 mL of 1-octadecene solution. Under the protection of argon, stir and heat to 140°C and keep it warm for 30min. After the rare earth particles are completely dissolved, cool naturally to room temperature.

[0033] (2) Then, successively dissolve 2.5mmol sodium oleate and 4mmol NH 4 10 mL of methanol solution of F was added dropwise to the reaction system, stirred and heated to 50 °C and kept for 60 min.

[0034] (3) Subsequently, under the protection of argon, the solution was stirred and heated to 260°C, kept for 30min, and then cooled to room temperature naturally.

[0035] (4) Centrifuge with a centrifuge, wash and centrifuge repeatedly with cyclohexane-ethanol three times, and finally disperse in cyclohexane or dry in an oven.

[0036] (5) Under the experimental conditions, uniformly dispersed pure phase β-NaYF with a size of 5.1 nm can be o...

Embodiment 3

[0038] (1) First, weigh 1mmol RECl of rare earth 3 ·6H 2 O (Y:Yb:Ho=75:20:5, molar ratio) was added to 6 mL of oleic acid and 15 mL of l-octadecene solution. Under the protection of argon, stir and heat to 155°C and keep it warm for 30 minutes. After the rare earth particles are completely dissolved, cool naturally to room temperature.

[0039] (2) Then, successively dissolve 2.5mmol sodium oleate and 4mmol NH 4 10 mL methanol solution of F was added dropwise to the reaction system, stirred and heated to 60°C and kept for 60 min.

[0040] (3) Subsequently, under the protection of argon, the solution was stirred and heated to 290°C, kept for 5 minutes, and then cooled to room temperature naturally.

[0041] (4) Centrifuge with a centrifuge, wash and centrifuge repeatedly with cyclohexane-ethanol three times, and finally disperse in cyclohexane or dry in an oven.

[0042] (5) Under the experimental conditions, uniformly dispersed pure phase β-NaYF with a size of 7.8nm can be...

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Abstract

The invention discloses a method for preparing a beta-NaYF4:Yb3+,RE3+(RE=Tm,Er,Ho) upconversion nanocrystal with the size of less than 8nm. Nucleation rate of a beta phase is accelerated and conversion from alpha-NaYF4 to beta-NaYF4 is efficiently promoted by introducing a sodium oleate ligand in a preparation process, so that reaction time for obtaining a pure phase beta-NaYF4: Yb3+,RE3+(RE=Tm,Er,Ho) upconversion nanocrystal can be shortened, and reaction temperature can be lowered. The prepared beta-NaYF4:Yb3+,RE3+(RE=Tm,Er,Ho) upconversion nanocrystal is small in size (4-8nm), good in dispersibility and free of an impure phase (alpha-NaYF4), the preparation method is simple, repeatability is high, and the beta-NaYF4:Yb3+,RE3+(RE=Tm,Er,Ho) upconversion nanocrystal has a wide application prospect.

Description

technical field [0001] The invention relates to the preparation of rare earth-doped up-conversion nanocrystals, in particular to a preparation of rare earth-doped β-NaYF below 8 nanometers 4 A method for upconversion nanocrystals, especially a β-NaYF with a size smaller than 8nm 4 :Yb 3+ , RE 3+ (RE=Tm, Er, Ho) up-conversion nanocrystal preparation method. Background technique [0002] Up-conversion luminescence is an anti-Stokes process that absorbs multiple low-energy photons and emits a high-energy photon. Up-conversion luminescent materials are a type of luminescent materials that can convert near-infrared light into visible light. Due to the very low phonon energy, β-NaYF 4 It is widely regarded as one of the most effective host materials capable of achieving highly efficient upconversion luminescence. In order to obtain α-NaYF-free 4 Pure phase of heterogeneous β-NaYF 4 , the preparation of the sample requires a higher reaction temperature and a longer reaction...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/02B82Y20/00B82Y40/00
Inventor 叶松李松王德平
Owner TONGJI UNIV
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