Method of preparing yttrium aluminium garnet fluorescent powder

A technology of yttrium aluminum garnet and a manufacturing method, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as insufficiency, difficulty in process control, and difficulty in ensuring the performance stability and consistency of final products, and achieves a solution to avoid pollution problems. Effect

Active Publication Date: 2007-08-08
JIANGSU BREE OPTRONICS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to realize the co-precipitation of all elements, there are considerable difficulties in process control, and it is difficult to guarantee the stability and consistency of the final product performance
[0005] In addition, there are wet chemical preparation methods such as Sol-Gel method and spray pyrolysis method, but there are still obvious deficiencies in process control and microscopic morphology.

Method used

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  • Method of preparing yttrium aluminium garnet fluorescent powder

Examples

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Comparison scheme
Effect test

Embodiment 1

[0016] (1) According to the stoichiometric ratio of the fluorescent powder, weigh the corresponding weight of ultrafine alumina powder, yttrium nitrate, cerium nitrate and gadolinium nitrate to prepare Al with a total concentration of 0.25, 0.73, 0.12, 0.28, 0.37 or 4.5M 2 o 3 suspension.

[0017] (2) Choose NaOH, NH 3 ·H 2 O and NH 4 HCO 3 At least one of them is formulated into a solution with a total concentration of 0.03, 0.05, 0.08, 1.25, 1.59 or 1.9M as a precipitating agent.

[0018] (3) Control the temperature of the prepared precipitation mother liquor within the range of 15, 25, 30, 42, 55 or 65°C, stir the suspension at a speed of 50, 90, 150, 260, 330 or 460rpm, and simultaneously mix the precipitant solution by 34 , 80, 240, 365, 470 or 500mL / min flow rate into the Al 2 o 3 In the suspension, when the pH value of the mother liquor reaches 6.8-11, stop the feeding process, and continue to keep warm and stir for 30, 60, 120, 180 or 240 minutes.

[0019] (4) ...

Embodiment 2

[0024] (1) Weigh Al 2 o 3 25.5g, Ce(NO 3 ) 2 ·6H 2 O 5.65g, Y 2 o 3 32.40g, the Y 2 o 3 Dissolve in 50ml of concentrated nitric acid with a concentration of 5M, heat and concentrate at 90°C to obtain white transparent Y(NO 3 ) 3 ·6H 2 O crystals, Al with deionized water 2 o 3 , Ce(NO 3 ) 2 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O was made into a 0.6M suspension and heated to 25°C. Then weigh NH 4 HCO3 120g is made into a 25% aqueous solution. While stirring the Al at 120rpm 2 o 3 suspension, while adding NH 4 HCO 3 The solution was added to Al at a flow rate of 25mL / min 2 o 3 In the suspension, when the pH value of the suspension reaches 8.2, stop feeding, continue to stir and keep warm for 120 minutes, centrifuge, wash with deionized water, dehydrate with absolute ethanol, and dry at 90°C. Then put it in a high-temperature reducing atmosphere furnace and heat it to 1350°C, keep it warm for 10 hours, pulverize the cooled powder, and sieve it to obtain the mole...

Embodiment 3

[0026] (1) Weigh Al 2 o 3 25.5g, Ce(NO 3 ) 2 ·6H 2 O4.78g, Y 2 o 3 33.08g, the Y 2 o 3 Dissolve in 50ml of concentrated nitric acid with a concentration of 5M, heat and concentrate at 90°C to obtain white transparent Y(NO 3 ) 3 ·6H 2 O crystals, Al with deionized water 2 o 3 , Ce(NO 3 ) 2 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O was made into a 0.6M suspension and heated to 25°C. Then weigh 20 g of NaOH to prepare a 10% aqueous solution. While stirring the Al at 120rpm 2 o 3 suspension, while adding NH 4 HCO 3 The solution was added to Al at a flow rate of 16mL / min 2 o 3 In the suspension, when the pH value of the suspension reaches 8.5, stop feeding, continue to stir and keep warm for 120 minutes, centrifuge, wash with deionized water, dehydrate with absolute ethanol, and dry at 90°C. Then put it in a high-temperature reducing atmosphere furnace and heat it to 1400°C, keep it warm for 6 hours, pulverize the cooled powder, and sieve it to obtain Y 2.89 Al 5 o...

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Abstract

The invention discloses a making method of fluorescent powder of yttrium aluminium garnet, which comprises the following steps: allocating certain quantity of alumina powder, yttrium nitrate, cerous nitrate and gadolinium nitrate into sediment mother liquid; allocating sediment agent solution through at least one of NaOH, NH3.H2O or NH3HCO3; maintaining sediment mother liquid temperature between 10 and 70 deg.c; stirring evenly; adding sediment agent solution into sediment mother liquid; stopping adding sediment agent when pH value is 6.8-11; insulating and stirring; separating solid from liquid of sediment mother liquid; washing solid through clean water; drying; adding fluoride in the powder as reacting adjuvant; placing blended powder into high-temperature stove; heating protected by gas; cooling; obtaining sintered fluorescent powder bulk; grinding; sieving; obtaining the product.

Description

1. Technical field [0001] The invention belongs to a method for manufacturing fluorescent materials, in particular to a method for manufacturing yttrium aluminum garnet fluorescent powder. 2. Background technology [0002] Prior Art: Yttrium Aluminum Garnet Y 3 Al 5 o 12 It is an important luminescent material matrix, which has the advantages of good chemical stability and radiation resistance. Among them, cerium-activated yttrium aluminum garnet YAG:Ce 3+ (YAG), with an excitation wavelength around 460nm, can effectively absorb the blue light emitted by GaN light-emitting diodes (LEDs), and its emission wavelength is around 540nm, which can be combined with the blue light of LEDs to obtain high-brightness white light. In order to further improve various performances of the phosphor, it is also necessary to dope it with other rare earth ions. This is also the only fluorescent material that can enter the practical stage at present. [0003] At present, this kind of phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/80
Inventor 何锦华梁超蒋建清董岩张超
Owner JIANGSU BREE OPTRONICS CO LTD
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