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Rare earth ion doped silicon oxynitride-based fluorescent powder, preparation method thereof and combustion synthesis device

A technology based on silicon oxynitride and rare earth ions, which is applied in chemical instruments and methods, luminescent materials, chemical/physical processes, etc., can solve the problems of low purity of synthetic products, unsuitable base phosphors, low utilization rate of raw materials, etc. Achieve the effects of short preparation time, uniform powder particle size distribution, and cost reduction

Active Publication Date: 2020-10-09
XINYU UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method solves the Si 2 N 2 The purity of the O synthesis product is not high, but there are also disadvantages such as complex process and low raw material utilization rate, so it is not suitable for doping Si with rare earth ions. 2 N 2 The preparation method of O-based fluorescent powder

Method used

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  • Rare earth ion doped silicon oxynitride-based fluorescent powder, preparation method thereof and combustion synthesis device
  • Rare earth ion doped silicon oxynitride-based fluorescent powder, preparation method thereof and combustion synthesis device
  • Rare earth ion doped silicon oxynitride-based fluorescent powder, preparation method thereof and combustion synthesis device

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Experimental program
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Effect test

Embodiment 1

[0035] According to the chemical formula Si (2-x) N 2 O:xRe(Re=Eu 2+ ), take x=0.01, Si:SiO 2 :Si 2 N 2 The molar ratio of O is 3:1:0.1, NH 4 The amount of Cl added is Si powder, SiO 2 Powder and Si 2 N 2 0.5% of the total mass of O powder, Eu 2 o 3 The amount of powder added is calculated according to the chemical formula. About 8.4 grams of Si powder, SiO 2 Powder 6 grams, Si 2 N 2 O powder 1g, NH 4 Cl powder 0.77g, Eu 2 o 3 0.7392 g of the powder was mixed and put into a ball mill tank for ball milling for 2 hours at a speed of 400 rpm, then dried at 80° C. for 8 hours and passed through a 100-mesh sieve. Put the pre-reaction powder 4 into the porous graphite crucible 3 containing the graphite rod 6, and put it into the reaction chamber 1 of the high-pressure combustion synthesis device. After the reaction chamber is evacuated until the air pressure is less than 10Pa, it is filled with 2.0MPa high-purity nitrogen gas with a purity of 99.999%. ignited by the...

Embodiment 2

[0038] According to the chemical formula Si (2-x) N 2 O:xRe(Re=Ce 3+ ), take x=0.005, Si:SiO 2 :Si 2 N 2 The molar ratio of O is 3:1:0.2, NH 4 The amount of Cl added is Si powder, SiO 2 Powder and Si 2 N 2 2% of the sum of the total mass of O powder, Ce 2 o 3 The amount of powder added is calculated according to the chemical formula. About 8.4 grams of Si powder, SiO 2 Powder 6 grams, Si 2 N 2 O powder 2 grams, NH 4 Cl powder 0.328g, Ce 2 o 3 0.3608 g of the powder was mixed and put into a ball mill jar for ball milling for 2 hours at a speed of 400 rpm, then dried at 80° C. for 8 hours and passed through a 100-mesh sieve. Put the pre-reaction powder 4 into the porous graphite crucible 3 containing the graphite rod 6, and put it into the reaction chamber 1 of the high-pressure combustion synthesis device. After the reaction chamber is evacuated until the air pressure is less than 10Pa, it is filled with 4.0MPa high-purity nitrogen gas with a purity of 99.999%. ...

Embodiment 3

[0040] According to the chemical formula Si (2-x) N 2 O:xRe(Re=Eu 2+ ), take x=0.001, Si:SiO 2 :Si 2 N 2 The molar ratio of O is 3:1:0, NH 4 The amount of Cl added is Si powder, SiO 2 Powder and Si 2 N 2 5% of the total mass of O powder, Eu 2 o 3 The amount of powder added is calculated according to the chemical formula. About 8.4 grams of Si powder, SiO 2 Powder 6 grams, NH 4 Cl powder 0.72g, Eu 2 o 3 0.0352 g of the powder was mixed and put into a ball mill tank for ball milling for 2 hours at a speed of 400 rpm, then dried at 80° C. for 8 hours and passed through a 100-mesh sieve. Put the pre-reaction powder 4 into the porous graphite crucible 3 containing the graphite rod 6, and put it into the reaction chamber 1 of the high-pressure combustion synthesis device. After the reaction chamber is evacuated until the air pressure is less than 10Pa, it is filled with 1.0MPa high-purity nitrogen gas with a purity of 99.999%. ignited by the bottom of the powder throu...

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Abstract

The invention discloses rare earth ion doped silicon oxynitride-based fluorescent powder and a preparation method and a combustion synthesis device thereof, and belongs to the technical field of fluorescent powder manufacturing. The chemical formula of the rare earth ion doped silicon oxynitride-based fluorescent powder is Si (2-x) N2O: xRe, and x is greater than or equal to 0.001 and less than orequal to 0.01. The used raw materials are cheap metal Si powder, SiO2 powder, NH4Cl powder and nitrogen, the raw materials are subjected to ball milling and then subjected to self-propagating combustion synthesis in a low-pressure nitrogen atmosphere, an external heat source is not needed, the preparation time is short, the energy consumption is low, the process is simple, and the efficiency is high so that the cost can be greatly reduced. A small amount of Si2N2O powder introduced into the raw materials can be used as a diluent to provide a nitrogen permeation channel for the nitridation reaction of the Si powder, and the combustion reaction temperature can be regulated and controlled to ensure that the synthesized Si2N2O product is not decomposed; and the introduced NH4Cl powder can beused as a catalyst to further promote nitridation of Si powder and regulate and control the combustion reaction temperature.

Description

technical field [0001] The invention belongs to the technical field of fluorescent powder manufacturing, and relates to a method for preparing fluorescent powder, in particular to a rare earth (Re) ion-doped silicon oxynitride (Si 2 N 2 O)-based phosphor powder and its preparation method and manufacturing equipment. Background technique [0002] In recent years, silicon-based nitride (oxide) phosphors have received extensive research and attention in the application field of white light LEDs due to their remarkable thermal stability, chemical stability, wide emission spectrum coverage and structural diversity. Such phosphors can generally be effectively excited by near-ultraviolet light or blue light, and exhibit special luminescent properties. At present, there are more and more mature silicon-based nitride phosphors doped with rare earth ions (such as Si 3 N 4 :Re(Re=Eu 2+ , Ce 3+ ,Tb 3+ )), silicon aluminum oxynitride phosphor (such as SiAlON:Re(Re=Eu 2+ , Ce 3+ ...

Claims

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Application Information

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IPC IPC(8): C09K11/59B01J19/08
CPCC09K11/7734C09K11/7721C09K11/7792C09K11/0883B01J19/087Y02B20/00
Inventor 史忠旗徐顺建刘桂武邹勇勇魏智磊
Owner XINYU UNIV
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