LiErF4-based core-shell structure up-conversion nanometer luminescent material and preparation method thereof

A nano-luminescent material and shell structure technology, applied in the direction of luminescent materials, nano optics, nanotechnology, etc., can solve the problem of uneven size of the core-shell structure, achieve uniform size, and solve the effect of uneven shell size

Inactive Publication Date: 2021-06-22
JILIN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The object of the invention is to provide a LiErF 4 Based on the core-shell structure up-conversion nano-luminescent material and its preparation method, so as to realize the high-efficiency luminescence, multi-wavelength excitation and excellent performance of single-wavelength emission of the up-conversion nano-material in the lithium system, and solve the problem of uneven core-shell structure size

Method used

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  • LiErF4-based core-shell structure up-conversion nanometer luminescent material and preparation method thereof
  • LiErF4-based core-shell structure up-conversion nanometer luminescent material and preparation method thereof
  • LiErF4-based core-shell structure up-conversion nanometer luminescent material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: Synthesis of LiErF 4 @LiYF 4

[0038] Step A: Synthesis of LiErF 4 bare core

[0039] (1) Weigh 1mmol of ErCl 3 ·6H 2 O (about 0.3810g) was added to a 50mL round-bottomed three-neck flask, and then 6mL oleic acid (OA) and 15mL 1-octadecene (ODE) were added;

[0040] (2) Turn on the stirring, feed nitrogen into the three-necked flask at room temperature, keep for 30 minutes, and remove the original oxygen in the flask;

[0041] (3) heating the reaction system in step (2) to 160° C., and then stirring for 30 minutes until the dissolution of the rare earth chloride powder in the solution is observed, and then cooling the reaction system to room temperature;

[0042] (4) Weigh 2.5mmol of LiOH (about 0.06g) and 4mmol of NH 4 F (about 0.148g) was added to a 20mL beaker, then 8mL of methanol was added, ultrasonicated for 10 minutes, dissolved and then added to the reaction system of step (3);

[0043] (5) The reaction system in step (4) is heated up to 70...

Embodiment 2

[0063] Embodiment 2: Synthesis of LiErF 4 @LiLuF 4

[0064] Step A: Synthesis of LiErF 4 bare core

[0065] (1) Same as Step A in Example 1.

[0066] Step B: Synthesis of LiLuF 4 shell precursor

[0067] (1) Weigh 2 mmol of lutetium trifluoroacetate (about 1.136 g) and 2 mmol of lithium trifluoroacetate (about 0.24 g) into a 50 mL three-necked flask;

[0068] (2) Measure 6mL of oleic acid, 6mL of oleylamine and 10mL of 1-octadecene into the three-necked flask of step (1), turn on the stirring, pass nitrogen into the three-necked flask at room temperature, and then raise the temperature to 65°C , until all the solids are dissolved;

[0069] (3) The temperature of the reaction system in step (2) is raised to 125° C. and kept for 30 minutes to remove oxygen and water in the system;

[0070] (4) The reaction system in step (3) was heated up to 290° C., reacted for 45 minutes, and cooled to room temperature after stopping heating;

[0071] (5) The reaction product of step ...

Embodiment 3

[0082] Embodiment 3: Synthesis of LiErF 4 @LiGdF 4

[0083] Step A: Synthesis of LiErF 4 bare core

[0084] (1) Same as Step A in Example 1.

[0085] Step B: Synthesis of LiGdF 4 shell precursor

[0086] (1) Weigh 2mmol gadolinium trifluoroacetate trihydrate (about 1.1g) and 2mmol lithium trifluoroacetate (about 0.24g) into a 50mL three-necked flask;

[0087] (2) Measure 6mL of oleic acid, 6mL of oleylamine and 10mL of 1-octadecene into the three-necked flask of step (1), turn on the stirring, pass nitrogen into the three-necked flask at room temperature, and then raise the temperature to 65°C , until all the solids are dissolved;

[0088] (3) The temperature of the reaction system in step (2) is raised to 125° C. and kept for 30 minutes to remove oxygen and water in the system;

[0089] (4) The reaction system in step (3) was heated up to 290° C., reacted for 45 minutes, and cooled to room temperature after stopping heating;

[0090] (5) The reaction product of step ...

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Abstract

The invention relates to a LiErF4-based core-shell structure up-conversion nanometer luminescent material and a preparation method thereof, and belongs to the technical field of luminescent material preparation. LiErF4 is used as a core, and on the basis, LiYF4, LiLuF4 and LiGdF4 inert shell layers are coated. A LiErF4 core material is cladded by adopting a thermal injection method, and the method comprises the following three steps: (1) firstly synthesizing a LiErF4 core raw material, mixing ErCl3.6H2O with a proper amount of LiOH and NH4F, and carrying out heating reaction to generate the core raw material; (2) preparation of three shell layer precursors: mixing corresponding trifluoroacetate with lithium trifluoroacetate, and carrying out heating reaction to generate the shell layer precursors; and (3) heating the LiErF4 core, injecting the synthesized shell layer precursor in batches at a high temperature, and reacting for a period of time to finally form a core-shell structure. The up-conversion nanoparticles with the core-shell structure synthesized by the invention are coated more uniformly, so that the intensity of up-conversion luminescence is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of luminescent material preparation, in particular to a LiErF 4 Based core-shell structure up-conversion nano-luminescent material and its preparation method. Background technique [0002] Lanthanide rare earth-doped upconversion nanoparticles have attracted extensive attention in recent years due to their excellent physicochemical properties. According to the current research, it has great potential in many fields such as solar energy utilization, luminescent display, and fluorescent security coding; especially because the up-conversion nanoparticles doped with lanthanide rare earths can be located in the biological spectral window region (650nm~1300nm ) near-infrared wavelength excitation, and up-convert the excitation light to ultraviolet, visible to near-infrared high-energy light emission (light in this waveband has the characteristics of deep tissue penetration and does not excite biological autofluor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/02B82Y20/00B82Y30/00
CPCB82Y20/00B82Y30/00C09K11/02C09K11/7705C09K11/7773
Inventor 卢革宇刘晓敏包浩强张玲卢阳
Owner JILIN UNIV
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