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A kind of preparation method of silicon oxynitride fluorescent powder

A technology of silicon oxynitride and silicon oxide, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as low luminous intensity, irregular shape, rapid growth and agglomeration

Inactive Publication Date: 2014-10-22
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the high temperature conditions for the synthesis of silicon oxynitride are generally greater than 1200 ° C, the general template such as SiO 2 Prone to rapid growth and agglomeration, resulting in poor dispersion of phosphor powder, irregular shape, and low luminous intensity

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  • A kind of preparation method of silicon oxynitride fluorescent powder
  • A kind of preparation method of silicon oxynitride fluorescent powder
  • A kind of preparation method of silicon oxynitride fluorescent powder

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[0043] The invention discloses a preparation method of silicon oxynitride fluorescent powder, comprising the following steps: step a) coating metal cations on the surface of nano microspheres, and obtaining a precursor powder after heat treatment, wherein the metal cations include matrix metal cations and luminescent metals Cation, the nanospheres are silicon oxide nanospheres, silicon nitride nanospheres, silicate nanospheres, core-shell hybrid nanospheres with silicon oxide as the shell, silicon nitride as the shell The core-shell hybrid nanospheres of the shell or the core-shell hybrid nanospheres with silicate as the shell; step b) coating the surface of the precursor powder with H 3 BO 3 , get H 3 BO 3 Coated precursor powder; step c) the H 3 BO 3 The coated precursor powder is reacted in a reducing atmosphere to obtain a h-BN coated precursor powder; step d) sintering the h-BN coated precursor powder at 1300-1650°C to obtain silicon oxide Nitride phosphor.

[0044]...

Embodiment 1

[0058] Will use 0.5g SiO with a diameter of about 280 nm prepared by 2 Ball, Sr 2+ and Eu 3+ The nitrate solution and a certain amount of urea are mixed together to prepare a uniform solution: the Sr in the solution 2+ (Eu 3+ ) concentration is 0.002mol / L, and the concentration of urea is 0.2mol / L;

[0059] Then the solution was heated to 85°C, kept at this temperature for 6 hours, then the obtained solution was suction filtered, dried, and sintered in the air at 500°C, and the sintered powder was mixed into 60°C H 3 BO 3 solution (dissolved with 2.5g H 3 BO 3 powder), then naturally lowered to 5°C under stirring, filtered, and dried;

[0060] Put the obtained powder into a BN boat, first raise the temperature to 1000°C for 2 hours in a 300ml / min ammonia gas flow, and then keep it at 1400°C for 8 hours to obtain spherical SrSi 2 o 2 N 2 :Eu 2+ Green fluorescent powder with a particle size of about 300nm.

[0061] Utilize XRD (X-ray diffractometer) to test and ana...

Embodiment 2

[0063] Will use 0.5g SiO with a diameter of about 280 nm prepared by 2 Ball, Sr 2+ and Eu 3+ The nitrate solution and a certain amount of urea are mixed together to prepare a uniform solution: the Sr in the solution 2+ (Eu 3+ ) concentration is 0.002mol / L, and the concentration of urea is 0.2mol / L;

[0064] Then the solution was heated to 85°C, kept at this temperature for 6 hours, then the obtained solution was suction filtered, dried, and sintered in the air at 500°C, and the sintered powder was mixed into 55°C H 3 BO 3 solution (dissolved with 3.0g H 3 BO 3 powder), then naturally lowered to 5°C under stirring, filtered, and dried;

[0065] Put the obtained powder into a BN boat, first raise the temperature to 1000°C for 2 hours in an ammonia gas flow of 300ml / min, and then keep it at 1400°C for 8 hours (the reducing atmosphere during the heat preservation is NH 3 and CH 4 mixed gas, and CH 4 Concentration of 3 ~ 5vol%), to obtain spherical Sr 2 Si 5 N 8 :Eu ...

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Abstract

The invention discloses a preparation method of silicon oxynitride fluorescent powder. The preparation method of the silicon oxynitride fluorescent powder comprises the following steps: coating the surface of a precursor powder with H3BO3; reacting the H3BO3-coated precursor powder in a reducing atmosphere to obtain h-BN-coated precursor powder; and sintering the h-BN-coated precursor powder to obtain the silicon oxynitride fluorescent powder. The surface of the precursor powder is coated with a h-BN protective layer, so that on the one hand, surface defects of nanospheres are reduced, thus making contribution to the improvement of the luminous intensity; and on the other hand, the h-BN protective layer is formed to avoid the agglomeration of the nanospheres, so as to ensure relatively good dispersion and regular shape of the prepared silicon oxynitride fluorescent powder. Experimental results show that the prepared fluorescent powder is excellent in conversion efficiency in a blue or near-ultraviolet waveband, excellent in color purity, high chemical stability, and small and uniform in grain size; and the preparation method is relatively low in sintering temperature, simple in process and easy in industrial continuous production and has a wide industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of luminescent materials, in particular to a preparation method of silicon oxynitride fluorescent powder. Background technique [0002] As an important part of white LED lighting technology and high-performance display technology, rare earth-doped silicon oxynitride phosphors have received extensive attention in recent years. First, the two-dimensional layered and three-dimensional network structure formed by its unique Si-(O, N) tetrahedral structure makes it have excellent thermodynamic stability and temperature quenching effect; second, it is compatible with O atoms Compared with N atoms, N atoms have a stronger electron expansion effect and crystal field effect, which makes the excitation wavelength range of phosphors red-shifted to the near ultraviolet-visible region; third, silicon oxynitride has very high chemical stability, and can resist water vapor and Various corrosive gases, stable in acidic and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/59C09K11/79
Inventor 徐鑫唐家业湛诚鞠立成
Owner UNIV OF SCI & TECH OF CHINA
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