Mn-doped aluminum nitride-based red phosphor powder and preparation method of red phosphor powder

A red phosphor and phosphor technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of high cost, complicated preparation process, restricting the wide application of red nitride phosphors, etc., and achieve low cost and good repeatability. , The effect of protecting the porous graphite crucible

Inactive Publication Date: 2012-12-19
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods either require high temperature, high pressure, long-term heat preservation, or pre-prepared precursors, or require post-treatment such as carbon removal, and at the same time add expensive rare earth elements, making the preparation process complicated and costly, which seriously restricts red nitrogen. Wide application of chemical phosphors

Method used

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  • Mn-doped aluminum nitride-based red phosphor powder and preparation method of red phosphor powder
  • Mn-doped aluminum nitride-based red phosphor powder and preparation method of red phosphor powder
  • Mn-doped aluminum nitride-based red phosphor powder and preparation method of red phosphor powder

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Composition of Al according to the chemical formula 1-x N:Mn x , take x=0.03, the mass ratio of Al powder and AlN powder is 4:6, that is, mix 7.762 grams of Al powder, 11.641 grams of AlN powder, and 0.629 grams of MnO and pass through a 100-mesh sieve. Put the mixed powder into a porous graphite crucible protected by a 3 mm thick graphite carbon felt, then put the porous graphite crucible into a high-pressure reaction vessel, and the high-pressure reaction vessel is evacuated to 10 -1 Pa, then fill with 1.0MPa purity and be 99.99% high-purity nitrogen; Light the igniter block that is placed on the bottom of the powder by the graphite paper strip and ignite, and the igniter block is a mixture of titanium powder and carbon powder in a 1:1 molar ratio The mixed powder is compressed, and the graphite paper belt is energized for 5 seconds under the condition of a energizing current of 24A and a voltage of 60V to make the combustion reaction occur. After the reaction, the ...

Embodiment 2

[0038] Composition of Al according to the chemical formula 1-x N:Mn x , take x=0.01, the mass ratio of Al powder and AlN powder is 6:4, that is, 11.570 grams of Al powder, 7.713 grams of AlN powder, 0.717 grams of MnCO 3 And pass through 200 mesh sieve. Put the mixed powder into a porous graphite crucible protected by a 2mm thick graphite carbon felt, then put the porous graphite crucible into a high-pressure reaction vessel, and the high-pressure reaction vessel is evacuated to 10 2Pa, and then fill with 3MPa purity of 99.999% high-purity nitrogen; ignite the igniter block placed at the bottom of the powder through the graphite paper strip to ignite, the igniter block is a mixture of titanium powder and carbon powder in a 1:1 molar ratio The graphite paper strip is energized for 10 seconds under the condition of energizing current of 20A and voltage of 70V to make the combustion reaction occur. After the reaction, the product in the porous graphite crucible was taken out a...

Embodiment 3

[0040] Composition of Al according to the chemical formula 1-x N:Mn x , take x=0.1, the mass ratio of Al powder and AlN powder is 3:7, that is, 4.716 grams of Al powder, 11.004 grams of AlN powder, 4.287 grams of MnO 2 Mix well and pass through a 300-mesh sieve. Put the mixed powder into a porous graphite crucible protected by a 4mm thick graphite carbon felt, then put the porous graphite crucible into a high-pressure reaction vessel, and the high-pressure reaction vessel is evacuated, and then filled with 0.5MPa nitrogen with a purity of 99.9%; The paper tape ignites the igniter block placed at the bottom of the powder to ignite. The igniter block is pressed from a mixture of titanium powder and carbon powder in a molar ratio of 1:1. Under the conditions of a current of 30A and a voltage of 50V The graphite paper strip was energized for 8 seconds to cause the combustion reaction to take place. After the reaction, the product in the porous graphite crucible was taken out an...

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Abstract

The invention discloses Mn-doped aluminum nitride-based red phosphor powder and a preparation method of the red phosphor powder. A chemical formula of the phosphor powder is Al1-xN:Mnx, wherein x is more than or equal to 0.01 and smaller than or equal to 0.1. The preparation method of the red phosphor powder comprises the steps of 1) weighing Al powders, AlN powders and compound powders containing Mn according to the weight of the target phosphor powder to be prepared, mixing uniformly and sieving, wherein the mass ratio of the Al powders to the AlN powders is 3:7-6:4; 2) adding the powders into a multi-hole graphite crucible, then putting into a high-pressure reaction container, vacuumizing, and introducing nitrogen; 3) igniting a ignition agent block at the powder bottom by lighting a graphite paper tape, and charging the graphite paper tape for 5-10s to initiate the combustion reaction under the conditions that the current is 20-30A and the voltage is 50-70V to obtain an incompact massive product; and 4) grinding, crushing and sieving the product to obtain the AlN:Mn2 red phosphor powder. The phosphor powder has the advantages that the light emitting efficiency is high, and the quality is stable. The preparation method has the advantages that the cost of raw materials is low, the process is simple, the speed is high, the needed production device is simple, the energy consumption is loss, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of fluorescent powder and its preparation, in particular to a Mn-doped aluminum nitride-based red fluorescent powder and a preparation method thereof. Background technique [0002] LED has attracted extensive attention as the most promising next-generation lighting method due to its advantages of energy saving, durability, and pollution-free. At present, there are many schemes for realizing white light LEDs, among which the combination of blue LED chips and yellow phosphor powder to realize white light emission is the most mature technical scheme for preparing white light LEDs. However, due to the lack of red light in the spectrum of the white light synthesized by this method, the color rendering index is low and the light efficiency is not high. One of the solutions is to coat green and red phosphors on the blue LED chip, and combine the blue light emitted by the chip with the green light and red light emi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
Inventor 史忠旗景瑞峰杨万利王继平刘桂武乔冠军杨建锋王红洁
Owner XI AN JIAOTONG UNIV
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