Nitrogen oxide phosphor powder and synthesis method thereof

A technology of nitrogen oxides and synthesis methods, which is applied in chemical instruments and methods, luminescent materials, sustainable buildings, etc., can solve the problems of reducing the luminous brightness of phosphors for LEDs, poor morphology of synthesized products, and low crystal phase purity of products. , to achieve smooth and improved crystallinity, reduce sintering temperature, and optimize crystal morphology.

Inactive Publication Date: 2013-02-06
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] MSi mentioned above 2 o 2 N 2 Oxynitride phosphors usually use a one-step synthesis method, and its manufacturing process requires high temperature and high pressure conditions. The synthesis conditions are relatively harsh, and the crystal phase purity of the obtained product is relatively low, resulting in a slightly lower brightness than other systems. Secondly, the shape of the synthetic product is The appearance is poor, and most of them are irregular flakes, resulting in scattering phenomenon, which greatly reduces the luminous brightness of phosphor powder for LED

Method used

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  • Nitrogen oxide phosphor powder and synthesis method thereof
  • Nitrogen oxide phosphor powder and synthesis method thereof
  • Nitrogen oxide phosphor powder and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The first step to synthesize the precursor Si of nitrogen oxide phosphor 2 N 2 O: Weigh SiO according to the stoichiometric ratio 2 60.1g, Si 3 N 4 140.31g, 3wt% flux ammonium chloride (NH 4 Cl) is mixed and fully ground (requires uniform mixing, the grinding time is 50min), then placed in an alumina crucible, placed in a tube furnace, sintered at 1500°C for 3 hours in a protective gas, and then naturally cooled to obtain Si 2 N 2 O, the protective gas is nitrogen, and the gas flow rate is 15ml / min.

[0030] The second step is in the front body Si 2 N 2 The matrix structure provided by O is doped with Sr and Eu elements to synthesize the oxynitride phosphor material Sr 0.96 Si 2 N 2 o 2 :0.04Eu: According to Sr 0.96 Si 2 N 2 o 2 : The stoichiometric ratio of 0.04Eu element will result in Si 2 N 2 After O is ground and sieved (150 mesh sieve), weigh 5g, then weigh SrCO 3 7.07g and Eu 2 o 3 0.351g, finally add 5wt% SrF2 Flux, the above-mentioned compo...

Embodiment 2

[0035] In order to show the advantages of preparing the nitrogen oxide phosphor material of the present invention, the first step of Example 2 is consistent with that of Example 1, and the parameters of the second step are mainly changed to compare with the examples.

[0036] The second step is in the front body Si 2 N 2 The matrix structure provided by O is doped with Ba, Sr and Eu elements to synthesize the oxynitride phosphor material Sr 0.4 Ba 0.58 Si 2 N 2 o 2 :0.02Eu: According to Sr 0.4 Ba 0.58 Si 2 N 2 o 2 : The stoichiometric ratio of 0.02Eu element will result in Si 2 N 2 After O is ground and sieved, weigh 5g, and then weigh BaCO 3 5.72g, SrCO 3 2.95g and Eu 2 o 3 0.176g, finally add 5wt% BaF 2 Flux, put the above ingredients into molybdenum crucible after grinding, move the crucible into high temperature tube furnace, 2 :H 2 =9:1 sintering at 1480°C for 4 hours with a gas flow rate of 25ml / min, then naturally cooled to room temperature and taken o...

Embodiment 3

[0039] The first step of embodiment 3 is consistent with that of embodiment 1, and the parameters of the second step are changed emphatically to contrast with each embodiment.

[0040] The second step is in the front body Si 2 N 2 The matrix structure provided by O is doped with Ca, Sr element and Eu element to synthesize the oxynitride phosphor material Ca 0.8 Sr 0.18 Si 2 N 2 o 2 :0.02Eu: According to Ca 0.8 Sr 0.18 Si 2 N 2 o 2 : The stoichiometric ratio of 0.02Eu element will result in Si 2 N 2 After O is ground and sieved, weigh 5g, and then weigh CaCO 3 4g, SrCO 3 1.33g and Eu 2 o 3 0.176g, finally add 5wt% SrF 2 Flux, put the above ingredients into molybdenum crucible after grinding, move the crucible into high temperature tube furnace, 2 :H 2 =9:1 sintering at 1480°C for 4 hours with a gas flow rate of 25ml / min, then cooled to room temperature and taken out.

[0041] Grind and sieve as required, wash and dry with dilute hydrochloric acid to obtain ni...

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Abstract

The invention relates to a nitrogen oxide phosphor powder and a synthesis method thereof. The nitrogen oxide phosphor powder is characterized in that the general chemical formula of the nitrogen oxide phosphor powder is Al-xByOzN2/3+4/3y-2/3z: xRE, wherein X is lager than or equal to 0 and smaller than 1.0, Y is larger than or equal to 1.0 and smaller than or equal to 3, Z is lager than 0 and smaller than or equal to 2.0; A represents at least one element of Be, Mg, Ca, Sr, Ba and Zn; B represents the element Si; and RE represents at least one element of Eu, Ce, Dy and Mn. The invention provides the novel method for preparing the nitrogen oxide phosphor powder for a light emitting diode (LED) by utilizing a two-step synthesis method. By using the novel method, the purity of the nitrogen oxide phosphor powder is increased to a large extent, the sintering temperature of the nitrogen oxide phosphor powder is further improved, crystal morphology of the nitrogen oxide phosphor powder is optimized, a particle surface of the nitrogen oxide phosphor powder is smooth, and the crystallinity is improved, so that the light emitting intensity of the nitrogen oxide phosphor powder is improved.

Description

technical field [0001] The invention relates to a nitrogen oxide fluorescent powder and a synthesis method thereof. Background technique [0002] Since Nichia released InGaN / Y in 1996 3 al 5 o 12 : Ce 3+ (referred to as YAG:Ce) phosphor single-chip white LED, and phosphor-converted white LED technology has become the mainstream of the market. The development of phosphors has evolved from less stable sulfides and halides to aluminates (Aluminate), silicates (Silicate), nitrides (Nitride) and nitrogen oxides ( Oxynitride) fluorescent materials, Nitride (Nitride) and Nitride (Oxy-nitride) are the most popular recently. [0003] In the 1980s, metal nitride (oxide) oxides were mostly used as structural or functional ceramics in the early days, and their application in white light LEDs was not noticed until recent years. Li et al. first developed MSi in 2005. 2 o 2 N 2 Fluorescent material and research on its luminescent properties, CaSi 2 o 2 N 2 :Eu emission peak at 5...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/59
CPCY02B20/181Y02B20/00
Inventor 赵莉苏醒宇
Owner IRICO
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