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Method for preparing rare earth doped aluminum nitride based blue fluorescent powder

A rare earth doping, aluminum nitride technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of high preparation cost, low production efficiency, limited application scope, etc., and achieve short preparation time, low cost, and improved efficiency. Effect

Inactive Publication Date: 2014-01-22
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high temperature required in the preparation process of these methods, the preparation cost is high and the production efficiency is low, which seriously limits its application range.

Method used

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  • Method for preparing rare earth doped aluminum nitride based blue fluorescent powder
  • Method for preparing rare earth doped aluminum nitride based blue fluorescent powder
  • Method for preparing rare earth doped aluminum nitride based blue fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] According to the rare earth-doped aluminum nitride-based blue phosphor chemical formula (1-x-y) AlN: xEu, ySi, take x=0.005, y=0.03, that is, the mole fraction of Eu is 0.5%, and the mole fraction of Si is 3%. Take aluminum powder, silicon powder and europium oxide powder as raw materials, the mass of ammonium fluoride is 20% of the total mass of raw materials, mix aluminum powder, silicon powder, europium oxide powder and ammonium fluoride powder and put them into a mortar and grind until uniform . Put the mixed powder into a BN (boron nitride) porcelain boat; then put the boron nitride porcelain boat into the tube furnace. 99.9% ammonia gas and nitrogen gas with a purity of 99.99% at a rate of 0.3L / min; raise the temperature of the tube furnace from room temperature to 1000°C at a rate of 5°C / min, and then at a rate of 3°C / min To 1450°C, keep warm at this temperature for 2 hours. After the sintering reaction, the product in the BN porcelain boat is taken out and gro...

Embodiment 2

[0024] According to the rare earth-doped aluminum nitride-based blue phosphor chemical formula (1-x-y) AlN: xEu, ySi, take x=0.008, y=0.03, that is, the mole fraction of Eu is 0.8%, and the mole fraction of Si is 3%. Take aluminum powder, silicon powder and europium oxide powder as raw materials, the mass of ammonium fluoride is 20% of the total mass of raw materials, mix aluminum powder, silicon powder, europium oxide powder and ammonium fluoride powder and put them into a mortar and grind until uniform . Put the mixed powder into a BN (boron nitride) porcelain boat; then put the boron nitride porcelain boat into the tube furnace, and after the tube furnace is evacuated to a pressure of less than 10Pa, the purity 99.9% ammonia gas and nitrogen gas with a purity of 99.99% at a rate of 0.1L / min; raise the temperature of the tube furnace from room temperature to 1000°C at a rate of 5°C / min, and then at a rate of 3°C / min To 1450°C, keep warm at this temperature for 2 hours. Aft...

Embodiment 3

[0026] According to the rare earth-doped aluminum nitride-based blue phosphor chemical formula (1-x-y) AlN: xEu, ySi, take x=0.005, y=0.05, that is, the mole fraction of Eu is 0.5%, and the mole fraction of Si is 5%. Take aluminum powder, silicon powder and europium oxide powder as raw materials, the mass of ammonium fluoride is 30% of the total mass of raw materials, mix aluminum powder, silicon powder, europium oxide powder and ammonium fluoride powder and put them into a mortar and grind until uniform . Put the mixed powder into a BN (boron nitride) porcelain boat; then put the boron nitride porcelain boat into the tube furnace. 99.9% ammonia gas and nitrogen gas with a purity of 99.99% at a rate of 1 L / min; the tube furnace is heated from room temperature to 1000 °C at a rate of 5 °C / min, and then to 1000 °C at a rate of 3 °C / min 1450°C, keep warm at this temperature for 2 hours. After the sintering reaction, the product in the BN porcelain boat is taken out and ground t...

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Abstract

The invention provides a method for preparing a rare earth doped aluminum nitride based blue fluorescent powder. Cheap aluminum powder, silicon powder and europium oxide powder are used as raw materials; in the process of sintering and heating, aluminum and silicon respectively melt into balls at 660 and 1400 DEG C, and the balls block the N atoms from entering into the metal, resulting in incomplete nitridation. The invention creatively uses ammonium fluoride to decompose and produce hydrogen fluoride and ammonia in the heating process, so as to destroy agglomerates formed by melted aluminum and silicon and ensure normal reaction; and the sintering temperature is greatly reduced, and the generated gas will volatile, without introducing impurities.

Description

technical field [0001] The invention belongs to the technical field of rare earth luminescent materials, and more specifically relates to a preparation method of rare earth doped aluminum nitride-based blue fluorescent powder. Background technique [0002] Light Emitting Diode (Light Emitting Diode) is an energy conversion device that can convert electrical energy into light energy. It has low operating voltage, low power consumption, stable performance, long life, strong shock resistance, vibration resistance, light weight, It has the advantages of small size, low cost, and fast luminous response. Especially in recent years, the rapid development of blue and ultraviolet LEDs has greatly expanded the scope of use of LEDs. [0003] At present, the method of realizing white light LED is mainly to coat phosphor powder on the blue light, violet light or ultraviolet light LED chip, and produce white light through the compounding of several colors. In recent years, nitrogen (oxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
Inventor 王超尹良君陈国璋简贤慕春红栾春红姜晶梁莹林
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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