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Core-shell structured silicate luminescent material and preparation method thereof

A technology of core-shell structure and luminescent materials, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., and can solve the problems of poor luminous intensity of phosphor powder, uneven particle distribution, and inconsistent particle size of powder, etc.

Inactive Publication Date: 2011-09-21
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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Problems solved by technology

[0002] Most of the current commercial luminescent materials are prepared by high-temperature solid-phase method. The high-temperature reaction consumes a lot of energy, the particle distribution is uneven, and the particle shape is different. Ball milling is required to obtain phosphors with a particle size of 2 to 8 microns. And the particle size of the powder is inconsistent, the shape is incomplete, resulting in uneven coating
People prepare phosphors by using sol-gel method, hydrothermal synthesis method, complex gel method and other methods. These methods can make up for the deficiency of high-temperature solid-phase synthesis method, but the luminous intensity of phosphor powder obtained by these methods is not as high as that of high temperature solid phase synthesis

Method used

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  • Core-shell structured silicate luminescent material and preparation method thereof
  • Core-shell structured silicate luminescent material and preparation method thereof

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preparation example Construction

[0018] The preparation method of the core-shell structure silicate luminescent material according to the embodiment of the present invention comprises the following steps:

[0019] use method coated SiO 2 Nanospheres, that is, after mixing ethanol, deionized water and ammonia water, adding tetraethyl orthosilicate to obtain SiO 2 nanospheres; again

[0020] According to the structural formula Ln 2-x SiO 5 :Tb x @SiO 2 Add the salt solution of Ln and Tb in the stoichiometric ratio of the corresponding elements, mix evenly, add dropwise oxalic acid solution to form a white precipitate, and then adjust the pH value of the reaction system to weak alkalinity with ammonia water, and then carry out formation, filtration, and dehydration in sequence. Wash the precipitate with ionic water and absolute ethanol, and finally dry to obtain the precursor;

[0021] The precursor is placed in a muffle furnace for heat treatment and reduction treatment, and then cooled to obtain the fi...

Embodiment 1

[0027] Preparation of Sc by Co-precipitation 1.95 SiO 5 :Tb 0.05 @SiO 2 :

[0028] Take 30mL absolute ethanol in a conical flask, then add 8mL deionized water and 10mL ammonia water, stir evenly, add 1.2mL tetraethyl orthosilicate while stirring, after reacting for 6 hours, add 7.8mL 1mol / LScCl 3 and 4mL 0.05mol / L TbCl 3 After stirring evenly, add 15mL of 1mol / L oxalic acid solution dropwise to form a white precipitate, then adjust the pH value to 8-9 with ammonia water, then stir for 3 hours, age, filter, and finally use deionized water and Washed three times with absolute ethanol, and dried to obtain the precursor. The precursor was heat treated in a muffle furnace at 1600 °C for 1 h, and then in a tube furnace at 95% N 2 +5%H 2 Sintering at 1000°C for 8 hours in reducing atmosphere, cooling to room temperature to obtain Sc 1.95 SiO 5 :Tb 0.05 @SiO 2 Luminescent material.

Embodiment 2

[0030] Preparation of Gd by Co-precipitation 1.80 SiO 5 :Tb 0.20 @SiO 2 :

[0031] Take 20mL absolute ethanol in a conical flask, then add 6mL deionized water and 3mL ammonia water, stir evenly, add 1.5mL tetraethyl orthosilicate while stirring, after reacting for 6 hours, add 3.6mL 2mol / LGd(NO 3 ) 3 and 4mL 0.20mol / L Tb(NO 3 ) 3After stirring the solution evenly, add 15mL of 1mol / L oxalic acid solution dropwise to form a white precipitate, then adjust the pH value to 8-9 with ammonia water, then stir for 3 hours, age, filter, and finally use deionized water and Washed three times with absolute ethanol, and dried to obtain the precursor. The precursor is placed in a muffle furnace for heat treatment at 900°C for 12 hours, then sintered in a muffle furnace at 1400°C for 4 hours in a carbon powder reducing atmosphere, and cooled to room temperature to obtain Gd 1.80 SiO 5 :Tb 0.20 @SiO 2 Luminescent material.

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Abstract

The invention provides a core-shell structured silicate luminescent material, the structural formula of which is Ln2-xSiO5:Tbx@SiO2. Wherein, Ln stands for at least one rare earth element, @ represents cladding, and x is greater than 0 and smaller than or equal to 0.5. The invention also provides a preparation method for the luminescent material, comprising the steps of: mixing ethanol, deionized water and ammoniacal liquor, and adding the mixture into ethyl orthosilicate so as to obtain SiO2 nanospheres, adding a salting solution of Ln and a salting solution of Tb, then adding oxalic acid, washing, precipitating and drying the mixed solution so as to obtain a precursor, and finally cooling the precursor after a heat treatment and a reduction treatment, thus obtaining a finished product. The core-shell structured silicate luminescent material obtained in the invention is characterized by controllable size and morphology, excellent luminescent property, and good stability, while the method has the advantages of simple preparation technology, short cycle of reaction, good reproducibility, low cost as well as wide prospect of manufacturing and application.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a core-shell structure silicate luminescent material and a preparation method thereof. Background technique [0002] Most of the current commercial luminescent materials are prepared by high-temperature solid-phase method. The high-temperature reaction consumes a lot of energy, the particle distribution is uneven, and the particle shape is different. Ball milling is required to obtain phosphors with a particle size of 2 to 8 microns. And the particle size of the powder is inconsistent, and the shape is incomplete, resulting in uneven coating. People prepare phosphors by using sol-gel method, hydrothermal synthesis method, complex gel method and other methods. These methods can make up for the deficiency of high-temperature solid-phase synthesis method, but the luminous intensity of phosphor powder obtained by these methods is not as high as that of high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/79
Inventor 周明杰王荣马文波
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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