Process of preparing fluorescent RE powder

A technology of rare earth phosphors and lanthanide rare earths, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of phosphor luminescence performance (poor brightness, difficulty in mixing raw materials uniformly, and lower reaction temperature, etc., to improve luminescence performance, Good product performance and low roasting temperature

Inactive Publication Date: 2009-04-29
PEKING UNIV
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Problems solved by technology

When using the solid phase reaction method to prepare phosphor, it is difficult to mix the raw materials evenly, the reaction temperature is high, and the product particle size is large, the particles are irregular, and the surface is uneven; the sol-gel method, spray drying method and combustion method are used to prepare fluorescent powder When powdering, the raw materials can be mixed evenly at the molecular level, and the reaction temperature can be reduced. The prepared phosphor has the characteristics of spherical, nearly spherical shape, controllable particle size, and smooth surface, but the luminous performance (brightness) of the phosphor poor

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  • Process of preparing fluorescent RE powder
  • Process of preparing fluorescent RE powder
  • Process of preparing fluorescent RE powder

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1, preparation Y 3 (Al, Ga) 5 o 12 :Tb green phosphor

[0028] The number of moles of raw materials used is as follows:

[0029] Yttrium oxide 27,

[0030] Aluminum hydroxide 54,

[0031] gallium oxide 18,

[0032] Terbium oxide 0.05.

[0033] The preparation process is as follows:

[0034] 1) In a pressure vessel, dissolve aluminum hydroxide and gallium oxide in excess hot nitric acid to make a nitrate solution, and dissolve yttrium oxide and terbium oxide in hot concentrated nitric acid in a heating and stirring device to make a nitrate solution. Mix the two solutions evenly to obtain a mixed solution, then adjust the pH value to 4 with ammonia water, add polyethylene glycol with a theoretical phosphor total mass of 150%, and stir at a constant temperature of 80° C. for 1.5 hours to form a gel;

[0035] 2) Heating the gel at 900°C for 1.5 hours to obtain a solid-phase calcined product;

[0036] 3) Grinding the solid-phase calcined product, and then...

Embodiment 2

[0040] Embodiment 2, preparation Y 3 Al 5 o 12 :Ce phosphor

[0041] The number of moles of raw materials used is as follows:

[0042] Yttrium oxide 23,

[0043] Aluminum hydroxide 76,

[0044] Cerium Oxide 1.

[0045] Its preparation steps are as follows:

[0046] 1) Dissolve aluminum hydroxide in excess hot nitric acid in a pressure vessel to make a nitrate solution, and dissolve yttrium oxide and cerium oxide in hot concentrated nitric acid in a heating and stirring device to make a nitrate solution; mix well and use urea Adjust the pH value to 5, add acrylamide with 200% of the total mass of the fluorescent powder, and stir at a constant temperature of 80°C for 10 hours to form a gel;

[0047] 2) The gel was heated at 500°C for 10 hours to obtain a solid-phase calcined product;

[0048] 3) After grinding the solid-phase pre-calcined product, add LiF with 5% of the theoretical phosphor mass, and burn it in a reducing atmosphere at 1200°C for 8 hours;

[0049] 4) Bo...

Embodiment 3

[0052] Embodiment 3, preparation Y 3 Al 5 o 12 : Ce, Gd phosphor

[0053] The number of moles of raw materials used is as follows:

[0054] Yttrium oxide 18.5,

[0055] Aluminum hydroxide 76,

[0056] Cerium oxide 1,

[0057] Gadolinium oxide 4.5.

[0058] Its preparation steps are as follows:

[0059] 1) In a pressure vessel, aluminum hydroxide is dissolved in excess hot nitric acid to make a nitrate solution, and in a heating and stirring device, yttrium oxide, gadolinium oxide and cerium oxide are dissolved in hot concentrated nitric acid to make a nitrate solution; After mixing the nitrate aqueous solution evenly, adjust the pH value to 3 with ammonia water, add citric acid with 300% of the total mass of phosphor powder, and stir at a constant temperature of 100°C for 2 hours to form a gel;

[0060] 2) The gel was heated at 400°C for 20 hours to obtain a solid-phase calcined product;

[0061] 3) Grinding the solid-phase calcined product, and then adding LiF and Ba...

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Abstract

The process of preparing fluorescent RE powder includes the following steps: 1. preparing mixture solution of yttrium nitrate 25-40 (in molar portions, the same below), aluminum nitrate 25-60, gallium nitrate 0-40, and lanthanon RE nitrate 0.03-10.0; regulating the solution pH to 2-8, adding gel forming agent and stirring at 80-120 deg.c for 1-24 hr to form gel; 2. heating the gel at 300-900 deg.c for 1.5-30 hr to obtain solid pre-baked product; and 3. grinding the solid pre-baked product, adding inorganic salt, igniting at 800-1600 deg.c in reducing atmosphere and washing to obtain the fluorescent RE powder. The preparation process of the present invention is simple, and has relaxed requirement in apparatus, high product performance and important industrial application value.

Description

technical field [0001] The invention relates to a method for preparing phosphor powder, in particular to a method for preparing rare earth phosphor powder. Background technique [0002] Rare earth luminescent materials have become supporting materials in information display, lighting source, optoelectronic devices and other fields. The high luminous intensity, good microscopic morphology and suitable particle size of phosphor can effectively improve the performance of devices. The commonly used phosphor is Y 3 (Al, Ga) 5 o 12 (Y 3 Al 5-x Ga x o 12 (x=0~3.0)) and other rare earth phosphors, whose main components are yttrium oxide or yttrium nitrate, aluminum oxide, aluminum nitrate or aluminum hydroxide, gallium oxide or gallium nitrate, etc., have good chemical and thermal stability, mainly It is used in color field emission display devices, projection TV, Head-up Display, etc. [0003] The preparation method of phosphor is the determining factor of phosphor luminous...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/78
Inventor 余泉茂荆西平
Owner PEKING UNIV
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