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Low-temperature solid-phase mengite fluorescent powder synthesizing method

A solid-phase synthesis, phosphor technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of large energy consumption and high requirements for heating equipment configuration.

Inactive Publication Date: 2004-01-28
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above preparation process consumes a lot of energy, and the configuration requirements of heating equipment in production are relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: monazite type La 0.64 Ce 0.30 Tb 0.06 PO 4 Preparation of green phosphor

[0025] reactant La 2 o 3 (lanthanum oxide), CeO 2 (ceria), Tb 4 o 7 (Terbium heptoxide) and (NH 4 ) 2 HPO 4 (Diammonium hydrogen phosphate) is accurately weighed according to the following molar ratio: La 2 o 3 : CeO 2 :Tb 4 o 7 :(NH 4 ) 2 HPO 4 = 0.32: 0.30: 0.015: 1, and mixed with template agent accounting for 50% (weight percent, Wt%) of the total amount of reactants, while adding grinding aid absolute ethanol, grinding in an agate mortar or ball mill. Dry the above-mentioned ground mixture and put it into a corundum crucible, compact it, put it into a heating container, heat it at 140°C, 160°C, 200°C, 300°C, and 400°C for 2 hours each, take it out, cool it, grind it, and refill it. Put it into a corundum crucible and compact it. Then put it into the heating container, under the reducing gas (N 2 90%+H 2 10%) in the presence of 750 ° C constant temperature hea...

Embodiment 2

[0027] Example 2 monazite configuration La 0.54 Gd 0.10 Ce 0.20 Tb 0.16 PO 4 green phosphor

[0028] reactant La 2 o 3 (lanthanum oxide), Gd 2 o 3 (gadolinium oxide), CeO 2 (ceria), Tb 4 o 7 (Terbium heptoxide) and (NH 4 ) 2 HPO 4 (Diammonium hydrogen phosphate) is accurately weighed according to the following molar ratio: La 2 o 3 :Gd 2 o 3 : CeO 2 :Tb 4o 7 :(NH 4 ) 2 HPO 4 = 0.27: 0.05: 0.20: 0.04: 1, and mix with the template agent that accounts for 10% ratio (Wt%) of above-mentioned reactant total amount, add grinding aid dehydrated alcohol simultaneously, grind in agate mortar or ball mill. Dry the above-mentioned ground mixture, put it into a corundum crucible, compact it, put it into a heating container, heat it at 140°C, 160°C, 200°C, 300°C, and 400°C for 1 hour, take it out and grind it, and then put it into the corundum Crucible, compacted. Then put it into a heating container, heat at 900°C for 1 hour, take it out while it is hot, cool and g...

Embodiment 3

[0030] Example 3 monazite configuration La 0.64 Ce 0.20 Tb 0.16 PO 4 green phosphor

[0031] Massive La 2 (C 2 o 4 ) 3 : CeO 2 :Tb 4 o 7 :(NH 4 ) 2 HPO 4 =0.32:0.20:0.04:1 Accurately weigh the reactant La 2 (C 2 o 4 ) 3 , CeO 2 , Tb 4 o 7 and (NH 4 ) 2 HPO 4 , and mixed with the templating agent accounting for 200% (Wt%) of the total amount of the above-mentioned reactants, while adding grinding aid absolute ethanol, grinding in an agate mortar or ball mill. Dry the above-mentioned ground mixture and put it into a corundum crucible, compact it, put it into a heating container, heat it at 140°C, 160°C, 200°C, 300°C, and 400°C for 1.5 hours, take it out and grind it, then put it into the corundum Crucible, compacted. Then put it into a heating container, heat it at a constant temperature of 680°C for 1 hour, take it out while it is hot, cool and grind, load the sample, and finally put it in the reducing gas (N 2 90%+H 2 10%) in the presence of 680 ° C c...

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PUM

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Abstract

On the basis of existent method the template agent is added, and a stage heating mode is adopted, and said invention also includes the steps of mixing, grinding, drying, charging mold, stage prebaking, ignition to make reduction and after-treatment to obtain various monazite type fluorescent powders under the condition of 600-900 deg.C.

Description

(1) Technical field [0001] The invention relates to a low-temperature solid-phase synthesis method for monazite-type fluorescent powder, which belongs to the field of chemical synthesis. (2) Technical background [0002] The molecular formula of monazite structure (with monoclinic structure) phosphor is: LnPO 4 :R 3+ (Rare earth phosphate Ln doped with rare earth luminescent ion R 3+ . R 3+ = Ce 3+ -Tb 3+ ;Ce 3+ ;Sm 3+ ; Yb 3+ ; Dy 3+ ;Eu 3+ Ho 3+ ;Er 3+ Wait. Ln = La and Gd). Different monazite-type phosphors have different uses, among which lanthanum cerium terbium phosphate (LaPO 4 : Ce 3+ , Tb 3+ ) is a green fluorescent powder, which has been used in low-voltage mercury-line fluorescent lamps and neon lamp manufacturing industries, as a green component in low-voltage tricolor energy-saving lamps or as a single-color advertising display material for outdoor neon lamps; while lanthanum cerium phosphate (LaPO 4 : Ce 3+ ) Ultraviolet fluorescent powder ha...

Claims

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Application Information

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IPC IPC(8): C09K11/08
Inventor 铁绍龙
Owner SOUTH CHINA NORMAL UNIVERSITY