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Preparation method of nitride-boride fluorescent powder material

A technology for phosphors and raw materials, applied in the field of preparation of rare earth or Mn2+ ion-activated nitrogen boride phosphor materials, can solve the problems of high price, harsh environment, unsuitable for industrial large-scale production, etc., and achieves low cost and short production cycle. , the effect of cheap raw materials

Active Publication Date: 2016-09-21
HUZHOU TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the raw materials used in the preparation process of this method are expensive nitrides, and the synthetic environment is relatively harsh (water and oxygen) so it is not suitable for industrial large-scale production

Method used

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  • Preparation method of nitride-boride fluorescent powder material
  • Preparation method of nitride-boride fluorescent powder material
  • Preparation method of nitride-boride fluorescent powder material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1, LiSr 4 (BN 2 ) 3 : Preparation of Cel mol%

[0048] Weigh 0.185g Li according to the stoichiometric ratio 2 CO 3 , 4.190g Sr(NO 3 ) 2 , 0.927g HBO 3 , 0.035g CeO 2 . Put the weighed raw materials into an agate grinder, add acetone and grind continuously until the acetone is completely volatilized, and all the raw materials are mixed uniformly. The mixture was then placed in a corundum crucible and sintered at 650°C for 3 hours under charcoal thermal conditions. The obtained sintered product was reground uniformly, then put into corundum crucible, sintered at 800℃ for 3 hours under the condition of carbon heat, and obtained LiSr after grinding 4 (BN 2 ) 3 : Celmol% phosphor. XRD powder diffraction indicated that pure LiSr was obtained 4 (BN 2 ) 3 structure( figure 1 ).

Embodiment 2

[0049] Example 2, LiSr 4 (BN 2 ) 3 : Preparation of Ce2mol%

[0050] Weigh 0.185g Li according to the stoichiometric ratio 2 CO 3 , 4.146g Sr (NO 3 ) 2 , 0.927g HBO 3 , 0.069g CeO 2 . Put the weighed raw materials into an agate grinder, add acetone and grind continuously until the acetone is completely volatilized, and all the raw materials are mixed uniformly. The mixture was then placed in a corundum crucible and sintered at 650°C for 3 hours under charcoal thermal conditions. The obtained sintered product was reground uniformly, then put into corundum crucible, sintered at 800℃ for 3 hours under the condition of carbon heat, and obtained LiSr after grinding 4 (BN 2 ) 3 : Ce2mol% phosphor. Use a fluorescence spectrometer to measure the excitation and emission spectra of phosphors, such as figure 2 shown. Under the excitation of near-ultraviolet light, the phosphors exhibit strong blue emission.

Embodiment 3

[0051] Example 3, LiSr 4 (BN 2 ) 3 : Preparation of Ce 0.5mol%, Tb2mol%

[0052] Weigh 0.185g Li according to the stoichiometric ratio 2 CO 3 , 4.169g Sr(NO 3 ) 2 , 0.927g HBO 3 , 0.017g CeO 2 , 0.083g Tb (NO 3 ) 3 4(H 2 O). Put the weighed raw materials into an agate grinder, add acetone and grind continuously until the acetone is completely volatilized, and all the raw materials are mixed uniformly. The mixture was then placed in a corundum crucible and sintered at 650°C for 3 hours under charcoal thermal conditions. The obtained sintered product was reground uniformly, then put into corundum crucible, sintered at 800℃ for 3 hours under the condition of carbon heat, and obtained LiSr after grinding 4 (BN 2 ) 3 : Ce2mol% phosphor. Use a fluorescence spectrometer to measure the excitation and emission spectra of phosphors, such as figure 2 shown. Under the excitation of near-ultraviolet light, the phosphors exhibit strong blue emission.

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Abstract

The invention relates to a preparation method of a nitride-boride fluorescent powder material. The preparation method is characterized in that common metal salt or oxide is used as the raw material, a high-temperature solid-phase method is used for preparation, the preparation process of nitride fluorescent powder is simplified, and production cost is lowered. The expression of the nitride-boride fluorescent powder material is AM4-4x(BN2):xD, wherein A is one or more of Li, Na, K, Rb and Cs; M is one or more of Mg, Ca, Sr and Ba, and D is one or more of Mn<2+>, Ce<3+>, Pr<3+>, Nd<3+>, Pm<3+>, Sm<3+>, Sm<2+>, Eu<3+>, Eu<2+>, Tb<3+>, Dy<3+>, Ho<3+>, Er<3+>, Tm<3+>, Yb<3+> and Yb<2+>. The preparation method specifically includes: weighing the raw materials of A, M and D and boric acid according to stoichiometric ratio, adding appropriate amount of acetone into the raw materials, and sufficiently grinding to obtain a mixture; performing heat preservation on the mixture for 1-5 hours in an environment of 400-650 DEG C and under reduction atmosphere; grinding and evenly mixing obtained preliminary-combustion substance, and performing heat preservation on the mixture for 1-8 hours in an environment of 700-900 DEG C to obtain the nitride-boride fluorescent powder material. The preparation method has the advantages that the method using a solid-phase synthesizing method is low in synthesizing temperature, simple in preparation process, low in cost, safe, reliable, short in production cycle and suitable for large-scale industrial production, and the prepared fluorescent powder is excellent in light-emitting efficiency.

Description

technical field [0001] The present invention relates to a kind of rare earth or Mn applied in the field of luminescence 2+ Preparation method of ion-activated boron nitride phosphor material. Background technique [0002] Semiconductor lighting or Light Emitting Diode (LED) is regarded as the fourth-generation lighting source due to its remarkable advantages of high efficiency, energy saving, environmental protection, long life and high luminous efficiency, and has received widespread attention and accelerated research and development around the world. At present, the most common method to realize white LED is to combine blue LED chips with yellow and red phosphors (such as YAG: Ce, CaAlSiN 3 : Eu 2+ ) or near-ultraviolet LED chips combined with red, green, and blue phosphors to achieve white light emission by adjusting the light output of different wavelength bands. Therefore, the development of three-primary phosphors suitable for excitation by blue light and near-ultra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/63
CPCC09K11/7715C09K11/7766
Inventor 罗文钦巫海燕李彬王永亚
Owner HUZHOU TEACHERS COLLEGE
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