High-brightness large-particle-size beta-SiAlON:Eu<2+> green emitting phosphor and preparation method thereof

A green phosphor, large particle technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of insufficient brightness, uneven particle size, small particle size, etc., to achieve uniform particles, wide process window, and large average particle size. Effect

Active Publication Date: 2017-01-04
HEBEI LIFU CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the objects of the present invention is to provide a high brightness, large particle size β-SiAlON:Eu 2+ Green phosphor to address existing β-SiAlON:Eu 2+ Green phosphor generally has the problems of insufficient brightness, small particle size and uneven particle size

Method used

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  • High-brightness large-particle-size beta-SiAlON:Eu&lt;2+&gt; green emitting phosphor and preparation method thereof
  • High-brightness large-particle-size beta-SiAlON:Eu&lt;2+&gt; green emitting phosphor and preparation method thereof
  • High-brightness large-particle-size beta-SiAlON:Eu&lt;2+&gt; green emitting phosphor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] β-SiAlON:Eu 2+ Preparation of green phosphor powder:

[0047] (1) Using α-Si 3 N 4 , AlN, Al 2 o 3 , Ga 2 o 3 、Eu 2 o 3 As raw material, according to the molar ratio of α-Si 3 N 4 :AlN:Al 2 o 3 : Ga 2 o 3 : Eu 2 o 3 =1.4:0.08:0.025:0.01:0.03 Weighing;

[0048] Note: Weighing of all the above raw materials must be carried out in the glove box N 2 Carried out under atmosphere (water content<1ppm, oxygen content<1ppm).

[0049] (2) Place the weighed raw material in a corundum mortar and grind it in one direction for 0.5h to fully mix the raw material, then pass through a 50-mesh sieve, and put it into a BN crucible.

[0050] (3) Primary sintering: Put the BN crucible into a high-temperature pressure sintering furnace, first pump the air with the mechanical pump to below 10Pa, turn on the molecular pump to pump air to the order of 10E-2, perform two times of air washing, and preheat to 500 °C , and then filled with N at a rate of 12MPa / h 2 :H 2 = 9:1 ra...

Embodiment 2～4

[0055] With reference to Example 1, change N in step (3) 2 / H 2 The ratio of the mixed atmosphere and other process conditions remained unchanged, and the brightness of the material after one sintering was measured, and the results are shown in Table 1. The primary material in the table refers to the primary sintered material obtained after one sintering, and the corresponding brightness is also the brightness of the primary sintered material.

[0056] Table 1:

[0057] Example β-SiAlON:Eu 2+ green phosphor h 2 :N 2 brightness Example 1 primary material 1:9 43.2 Example 2 primary material 1:19 32.5 Example 3 primary material 1:4 12.5 Example 4 primary material Pure N 2 23.4

Embodiment 5～9

[0059] Referring to Example 1, only the primary sintering time in step (3) was changed, and other parameters and conditions remained unchanged, and the brightness of the material after primary sintering was measured, and the results are shown in Table 2. The primary material in the table refers to the primary sintered material obtained after one sintering, and the corresponding brightness is also the brightness of the primary sintered material.

[0060] Table 2:

[0061] Example β-SiAlON:Eu 2+ green phosphor Primary sintering time (h) brightness Example 1 primary material 6 43.2 Example 5 primary material 1 5.6 Example 6 primary material 4 23.5 Example 7 primary material 8 44.1 Example 8 primary material 10 32.5 Example 9 primary material 12 30.8

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Abstract

The invention relates to a high-brightness large-particle-size beta-SiAlON:Eu<2+> green emitting phosphor and a preparation method thereof. The chemical general formula of the phosphor is Sia(AlxGa1-x)bOcNd:Eue<2+>, wherein 0.4<=a<=0.5, 0.01<=b<=0.02, 0.006<=c<=0.02, 0.47<d<=0.664, 0<e<=0.010, and 0<x<1; and the phosphor is prepared through double sintering, and the second sintering is performed by mixing a first sintering material obtained by first sintering and raw materials and then sintering. The beta-SiAlON:Eu<2+> green emitting phosphor prepared by the invention has the advantages of uniform particles, large average particle size and high luminescent intensity, has a wide prospect in preparation of white light LEDs (light-emitting diode), and is further mainly used as a backlight liquid crystal display (LCD) in a semiconductor light-emitting device. The process method provided by the invention is suitable for large-scale industrial production, and can realize preparation of the beta-SiAlON:Eu<2+> green emitting phosphor with expected particle size and uniformity, high brightness and narrow peak by controlling raw material proportioning and temperature regulation.

Description

technical field [0001] The present invention relates to a kind of sialon type green fluorescent powder and its preparation method, specifically a kind of high brightness, large particle size β-SiAlON:Eu 2+ Green fluorescent powder and its preparation method. Background technique [0002] SiAlON phosphor is a kind of nitrogen oxide phosphor mainly including four chemical elements Si, Al, O, and N. Its crystal structure is similar to that of Si 3 N 4 similar. In the Si-Al-O-N quaternary system, due to the cation M(Si 4+ 、Al 3+ ) and anion X (N, O) in different proportions, the solid solutions formed are also different, mainly β-SiAlON, α-SiAlON, O-SiAlON, X-SiAlON and AlN polytypes (8H, 12H, 15R, 21R, 27R, etc.). The general formula of β-SiAlON is Si 6-Z al Z o Z N 8-Z , where 0<Z≤4.2, the β-SiAlON observed under the scanning electron microscope is a typical hexagonal columnar crystal, which is larger than β-Si 3 N 4 The crystal is coarse, so the toughness and s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
CPCC09K11/0883C09K11/7734
Inventor 杨志平王海龙赵金鑫
Owner HEBEI LIFU CHEM TECH
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