Up-conversion luminescent material as well as preparation method and application thereof

A luminescent material and chemical technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of low luminous efficiency and large size, and achieve the effects of high luminous efficiency, small size and stable performance

Inactive Publication Date: 2015-03-11
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the object of the present invention is to provide an up-conversion luminescent material and its preparation method

Method used

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  • Up-conversion luminescent material as well as preparation method and application thereof
  • Up-conversion luminescent material as well as preparation method and application thereof
  • Up-conversion luminescent material as well as preparation method and application thereof

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preparation example Construction

[0041] The present invention also provides a preparation method of the up-conversion luminescent material: a solvothermal method using octadecene as a solvent and oleic acid as a complexing agent. The method has a low reaction temperature, is easy to operate, and has no pollution to the environment, and specifically includes the following steps :

[0042] 1) According to the stoichiometric ratio of each element in the general chemical formula (1), weigh the 3+ compounds containing R 3+ Compounds containing Yb 3+ compounds and containing M 3+ The compound is added in the three-necked flask;

[0043] 2) After adding oleic acid and octadecene into the three-necked flask at a volume ratio of 2:5, under nitrogen or inert gas conditions, heat to 140-180°C for 30-60 minutes, then cool to 50°C, Form solution A;

[0044] 3) According to F in the general chemical formula (1) - and Na + The stoichiometric ratio of NH 4 F and excess NaOH are dissolved in methanol to obtain solutio...

Embodiment 1

[0054] β-NaLu 0.78 Yb 0.2 Er 0.02 f 4 preparation of

[0055] According to the chemical formula NaLu 0.78 Yb 0.2 Er 0.02 f 4 The stoichiometric ratio of each element in, respectively weighed 0.2195g LuCl 3 , 0.0559g YbCl 3 and 0.0055g ErCl 3 , was added to a 100ml three-necked flask; then 6ml of oleic acid and 15ml of octadecene were added to the three-necked flask, and under the protection of nitrogen, the solution was heated to 140°C for 30 minutes, then cooled to 50°C to form solution A; 0.148g NH 4 F. Dissolve 0.1g NaOH into 10ml of methanol solution and mix well, then slowly inject into solution A, keep the temperature at 50°C for 30 minutes to evaporate the methanol; continue to heat the solution to 300°C for 1.5 hours, then cool to room temperature, Form nanocrystals; precipitate nanocrystals with excess absolute ethanol, centrifuge 3 times at a speed of 5000 rpm, and obtain a white paste that is β-NaLu 0.78 Yb 0.2 Er 0.02 f 4 Up-converting luminescent ma...

Embodiment 2

[0061] β-NaLu 0.58 Y 0.2 Yb 0.2 Er 0.02 f 4 preparation of

[0062] According to the chemical formula NaLu 0.58 Y 0.2 Yb 0.2 Er 0.02 f 4 The stoichiometric ratio of each element in , respectively weighed 0.1633gLuCl 3 , 0.0391g YCl 3 , 0.0559g YbCl 3 and 0.0055g ErCl 3 , was added to a 100ml three-necked flask; then 6ml of oleic acid and 15ml of octadecene were added to the three-necked flask, and under the protection of nitrogen, the solution was heated to 140°C for 30 minutes at a constant temperature, and then cooled to 50°C to form solution A; 0.148g NH 4 F. Dissolve 0.1g NaOH in 10ml of methanol solution and mix well, then slowly inject into solution A, and keep the temperature at 50°C for 30 minutes to evaporate the methanol; continue to heat the solution to 300°C for 1.5 hours, then cool to room temperature , to form nanocrystals; precipitate nanocrystals with excess absolute ethanol, and centrifuge 3 times at a speed of 5000 rpm to obtain a white paste, w...

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Abstract

The invention discloses an up-conversion luminescent material as well as a preparation method and the application thereof. The material is a nanoscale hexagonal disk-shaped fluoride, and has the following chemical general: NaLu1-x-y-zRxYbyMzF4, wherein R is a rare earth element Y or any composition of the Y, Gd and La; M is one of or any composition of the rare earth elements Ho, Er and Tm; x, y and z meet the following conditions that x is greater than or equal to 0 and less than or equal to 0.5, y is greater than or equal to 0.1 and less than or equal to 0.5, and z is greater than or equal to 0 and less than or equal to 0.1; the material is prepared by a solvothermal method, which takes octadecene as a solvent and takes oleic acid as a complexing agent, and can be used on the aspects of storage, transmission, optical display, infrared detection, fluorescent falsification-preventing, fluorescence probe, biosensor, and bio-imaging; the material is stable in performance and regular in morphology; the particle size is obviously smaller than that of beta-NaLuF4 synthesized under the same condition; the luminous intensity is higher than that of the up-conversion luminescent materials of beta-NaYF4 and beta-NaLuF4 which is synthesized under the same condition; the up-conversion luminescent material has the advantages of small size, high luminous efficiency and the like.

Description

technical field [0001] The invention relates to the field of luminescent materials, and in particular provides an up-conversion luminescent material and its preparation method and application. Background technique [0002] The up-conversion luminescence of rare earth ions refers to the phenomenon that when a sample doped with rare earth ions is irradiated with excitation light with a longer wavelength, light with a wavelength smaller than that of the excitation light is emitted. Up-conversion luminescent materials have broad application prospects in data storage and transmission, light display, infrared detection, fluorescent anti-counterfeiting, fluorescent probes, biosensors, bioimaging, solar cells and other fields. Compared with traditional down-conversion fluorescent materials (such as quantum dots, organic dyes, etc.), up-conversion materials have many advantages, such as low toxicity, high photostability, low background fluorescence, high color purity and long life. ...

Claims

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Application Information

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IPC IPC(8): C09K11/85
Inventor 张家骅相国涛张霞郝振东潘国徽
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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