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Preparation method and application of red phosphor and its carbothermal reduction nitriding
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A technology of red fluorescence and phosphor, applied in chemical instruments and methods, luminescent materials, semiconductor devices, etc., can solve the problems of unfavorable industrial production, increase of synthesis cost, high synthesis temperature, etc., and achieve easy mass production, lower color temperature, and synthesis The effect of low temperature
Active Publication Date: 2016-03-23
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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But in above all patent document reports, main synthetic raw material all uses the nitride (especially Ca 3 N 2 ,Sr 3 N 2 etc.), which are not only expensive, but also inconvenient to operate. In addition, the synthesis temperature is relatively high and a certain gas pressure is required, which increases the synthesis cost and is very unfavorable for large-scale industrial production.
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[0075] (Preparation method of phosphor)
[0076] The phosphor of the present invention can be prepared by carbothermal reduction nitriding method, which can include batching, mixing, sintering and post-treatment processes.
[0077] 1. Ingredients
[0078] As a Ca source, CaCO can be used 3 and / or CaO and / or CaC 2 o 4 . As Sr, SrCO can be used 3 and / or SrO. As the Si source, Si can be used 3 N 4 and / or SiO 2 . As the Al source, AlN can be used. As the A source, a metal element, an oxide, a nitride, a fluoride, a chloride, a carbonate, or an oxynitride of the A element can be used.
[0079] Weigh the above-mentioned raw materials according to the stoichiometric ratio of the chemical formula of the phosphor, and add reducing agent carbon powder therein. The molar ratio of the amount of carbon powder added to the oxygen element in the raw material (the carbonate decomposed during the heating process is calculated based on the oxides generated after decomposition) can be ...
Embodiment 1~7
[0104] Formulation design: according to the chemical formula Ca 0.98 Eu 0.02 Al 1-4δ / 3 Si 1+δ N 3 (Ca 1-x-y Sr y Eu x Al 1-4δ / 3 Si 1+δ N 3-2z / 3 o 3z / 2 , x=0.02, y=0, z=0) designed 7 formulations (δ=0, 0.06, 0.12, 0.18, 0.24, 0.30, 0.36).
Embodiment 8~13
[0106] Formulation design: according to the chemical formula Ca 1-x Eu x Al 0.76 Si 1.18 N 3 (Ca 1-x-y Sr y Eu x Al 1-4δ / 3 Si 1+δ N 3-2z / 3 o 3z / 2 , δ=0.18, y=0, z=0) designed 6 recipes (x=0.01, 0.02, 0.03, 0.05, 0.08, 0.1).
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Abstract
The invention relates to a red fluorophor as well as a carbothermal reduction nitridation preparation method and an application of the red fluorophor. The red phosphor is formed by carrying out solid solution on an activator A in the Ca[1-y]SryAlaSibNcOd substrate having the same crystal structure as that of the CaAlSiN3 crystalline phase, the chemical formula of red phosphor is Ca[1-vx / 2-y]SryAxAlaSibNcOd, wherein x is greater than 0 and less than or equal to 0.2, y is equal to or greater than 0 and less than or equal to 0.8, a is equal to or greater than 0.52 and less than or equal to 1, b is equal to or greater than 1 and less than or equal to 1.36, c is greater than 2.85 and less than or equal to 3 and d is equal to or greater than 0 and less than or equal to 0.2, the element A is at least one element selected from Eu, Mn, Yb, Ce, and Tb and v is representative of the electrovalence of the activator A ion and the preparation method of the red fluorophor comprises the following steps of maintaining CaCO3 powder and / or CaO powders and / or CaC2O4 powder, SrCO3 and / or SrO powder, Si3N4 powder and / or SiO2 powder, AlN powder, and single metal, oxide, nitride, fluoride, chloride, carbonate and / or nitrogen oxide powder of element A as starting materials in the presence of carbon powder as a reducing agent at a mixed atmosphere nitrogen and hydrogen or a mixed atmosphere of nitrogen, hydrogen and ammonia at a temperature range of 1550-1650 DEG C and sintering.
Description
technical field [0001] The present invention relates to a kind of with and CaAlSiN 3 Preparation of nitrogen (oxygen) oxide red phosphor with the same crystal structure by carbothermal reduction nitriding method and its application in lighting equipment and other fields. More specifically, the present invention relates to the low-cost preparation of an excellent nitrogen (oxide) oxide red phosphor and its use in the fields of white LED lighting fixtures can significantly improve its color characteristics and achieve warm white light. Background technique [0002] Compared with traditional light sources, LED has the advantages of high luminous efficiency, energy saving, environmental protection, long life, small size, fast response, high reliability, and no radiation, and its proportion in the global lighting market is increasing day by day. , Fluorescent lamps and high-intensity discharge lamps (High Intensity Discharge, HID) after the fourth generation of lighting sources ...
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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64H01L33/50
CPCY02B20/00
Inventor 刘学建李淑星黄政仁姚秀敏
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI