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Method for preparing ball milling free spherical crystal type fluorescent powder

A fluorescent powder and ball-milling-free technology, which is applied in the preparation of blue fluorescent powder, yttrium aluminum garnet fluorescent powder and tricolor green, can solve the problems of reducing particle size, large powder particles, long heat preservation time, etc., and achieve sintering hardness Reduced, complete crystal structure, small central particle size

Inactive Publication Date: 2008-03-26
湖南信多利新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main advantages of this method are: the crystal quality of the microcrystal is excellent, the surface defects are few, the luminous efficiency is high, the process is easy to operate, and it is beneficial to industrial production; Burn once in the left and right hydrogen reduction furnaces, the holding time is longer (more than 3h), the requirements for equipment are high, the generated powder particles are large and easy to agglomerate, and the particle size needs to be reduced by ball milling to meet the coating requirements of the lamp tube
Ball milling is easy to destroy the crystal form of the luminescent body, reduce the luminescent performance, and the particle size distribution is uneven, and many impurities or impurity phases are produced

Method used

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  • Method for preparing ball milling free spherical crystal type fluorescent powder
  • Method for preparing ball milling free spherical crystal type fluorescent powder
  • Method for preparing ball milling free spherical crystal type fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1, the process flow of the YAG fluorescent powder of the present invention is: batching-→jet milling-→mixing to make uniform-→high temperature pre-burning (1400-1450 degrees)-→detection-→crushing, washing through a 400-mesh wet sieve -→centrifugation-→drying-→airflow crushing-→100 mesh sieving-→testing-→low temperature reduction (1150-1250 degrees)-→testing-→crushing, coarse sieving-→washing, wet sieving, centrifugation, drying Drying-→100 mesh screening-→comprehensive testing-→finished product.

[0040] The pretreatment of each raw material in the preparation process, the intermediate treatment after high temperature pre-calcination, the firing temperature and the post-treatment method are the key factors affecting the product quality. BaF used as flux 2 、H 3 BO 3 Dry ball milling, passing through a 200-mesh sieve; according to chemical formula Y 3-3x al 5 o 12 : xCe stoichiometric ratio relationship, weighing alumina, yttrium oxide, cerium oxide and o...

Embodiment 2

[0042] The technological process of the three-color green fluorescent powder of the present invention is: batching-→airflow crushing-→mixing to make uniform-→high temperature pre-burning (1400-1450 degrees)-→detection-→crushing, washing through a 400-mesh wet sieve-→ Centrifugation-→drying-→airflow crushing-→100 mesh sieving-→testing-→low temperature reduction (1150-1250 degrees)-→testing-→crushing, coarse sieving-→washing, wet sieving, centrifugation, drying- →100 mesh screening-→comprehensive testing-→finished product.

[0043] BaF used as flux 2 Dry ball milling, passing through a 200-mesh sieve; according to the chemical formula MgAl 11 o 19 : Ce, Tb stoichiometric ratio relationship, weigh alumina, terbium oxide, cerium oxide, magnesium oxide and other raw materials, add flux BaF accounting for 1 to 5% of the chemical formula 2 , to obtain the mixture; use a supersonic jet mill to crush the mixture so that the central particle size is 4.0±0.5um; put the crushed mixture...

Embodiment 3

[0045] The technological process of the three-color blue fluorescent powder of the present invention is: batching-→airflow crushing-→mixing to make uniform-→high temperature pre-burning (1400-1450 degrees)-→detection-→crushing and washing through a 400-mesh wet sieve- →centrifugation-→drying-→airflow crushing-→100 mesh sieving-→detection-→low temperature reduction (1150-1250 degrees)-→detection-→crushing, coarse sieving-→washing, wet sieving, centrifugation, drying -→100 mesh screening-→comprehensive testing-→finished product.

[0046] BaF used as flux 2 、H 3 BO 3 Dry ball milling, passing through a 200-mesh sieve; according to the chemical formula Ba, MgAl 10 o 17 : Eu, Mn stoichiometric ratio relationship, weigh aluminum oxide, europium oxide, magnesium oxide, barium carbonate, manganese carbonate and other raw materials, add flux BaF accounting for 1 to 5% mole of the chemical formula 2 、H 3 BO 3 , to obtain the mixture; use a supersonic jet mill to crush the mixture...

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Abstract

The no ball milling spherical crystal phosphor powder preparing process belongs to the field of light-emitting RE material technology and relates to preparation process of YAG phosphor powder and green-blue phosphor powder for LED. By using yttria, cerium oxide, magnesia, barium carbonate, manganese carbonate, barium fluoride and other materials and through one improved high temperature solid phase process, phosphor powder of 5.0-6.0 micron size for use in making LED may be prepared directly without need of ball milling. The present invention has simple technological process, low preparation cost, high yield, capacity of obtaining high purity and high performance phosphor powder and other advantages.

Description

technical field [0001] The invention relates to a preparation method of rare earth luminescent material fluorescent powder, in particular to a preparation method of yttrium aluminum garnet (YAG) fluorescent powder and three primary color green and blue fluorescent powders for LED. Background technique [0002] The preparation method of the yellow YAG phosphor powder for white light LED is similar to that of the green and blue phosphor powders of the three primary colors. There are many kinds of existing preparation techniques, such as co-precipitation method, sol-gel method, citric acid-gel method, polymer network gel method, and combustion method. Although the synthesis temperature of these methods is low, the product phase purity is high , excellent chemical uniformity and small particle size, but the synthetic material has low luminous efficiency, poor crystallization, difficult to control the crystal shape, needs to be filtered and cleaned many times, the process is comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/00
Inventor 刘清玲蒋葵明
Owner 湖南信多利新材料有限公司
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