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Microwave sintering process for RE luminophor material

A rare earth fluorescent and bulk material technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of high calcination energy consumption, large grain size of calcined products, lack of general adaptability, etc., to shorten the calcination time, The effect of fast crystal formation, energy saving and environmental pollution

Active Publication Date: 2009-06-10
艾柯谷生态农业发展(河北)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The high-temperature electric furnace firing method is a traditional method for preparing rare earth luminescent materials. The main disadvantages are: (1) The fired product has large grains, high density, and high hardness, and ball milling is usually required; (2) The firing temperature is high and the reaction time is high. It takes a long time to cool the product, and the product often has a small amount of mesophase in addition to the main crystal phase; (5) Calcination at a higher temperature consumes a lot of energy.
The above-mentioned burning method lacks universal adaptability in the reduction method

Method used

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  • Microwave sintering process for RE luminophor material
  • Microwave sintering process for RE luminophor material

Examples

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Effect test

example 1

[0022] Take the stoichiometric ratio as Ba 3 MgSi 1.9 Al 0.1 o 8 :Eu 0.02 , Mn 0.1 100 grams of xerogel powder samples were placed in a 500 ml corundum crucible containing 99% alumina, opened without a cover, and placed in a muffle furnace with a maximum temperature of 1200 °C; the temperature was controlled at 1000 °C for constant temperature heating Pre-burn for 60 minutes, take it out after cooling; after pre-burning, put the crucible with the sample into the microwave oven without a cover, and put 95N into the reaction chamber 2 +5%H 2 reducing gas, start the power of the microwave oven, control the power of the microwave oven to 4 kilowatts, and burn for 2 hours; turn off the power of the microwave oven and the reducing gas, and naturally cool to room temperature to obtain the phosphor product. attached figure 1 for getting Ba 3 MgSi 1.9 Al 0.1 o 8 :Eu 0.02 , Mn 0.1 X-ray diffraction analysis spectrum of phosphor products.

example 2

[0024] Take the stoichiometric ratio as Ba 3 MgSi 1.9 Al 0.1 o 8 :Eu 0.02 , Mn 0.1 100 grams of xerogel powder samples were placed in a small corundum crucible with a volume of 500 milliliters containing 99% alumina, opened without a cover, and placed in a muffle furnace with a maximum temperature of 1200 ° C; the temperature was controlled at 700 Heating at a constant temperature of ℃ for 120 minutes for pre-burning, and taking it out after cooling; the corundum crucible with the sample after pre-burning is opened without a cover, and transferred to a large corundum crucible in a microwave oven, and activated carbon material is filled between the two crucibles. Put a ceramic cover on top; connect the furnace to the atmosphere, turn on the power of the microwave oven, control the power of the microwave oven to 2 kilowatts, and burn for 4 hours; turn off the power of the microwave oven, and cool naturally to room temperature to obtain the phosphor product. The X-ray diffra...

example 3

[0026] Take the stoichiometric ratio as (Sr, Ca) 2 MgSi 2 o 7 :Eu 2+ , Dy 3+ 100 grams of xerogel powder samples were placed in a small corundum crucible with a volume of 500 milliliters containing 99% alumina, and placed in a muffle furnace with a maximum temperature of 1200 ° C; the temperature was controlled at 800 ° C and heated for 180 minutes Carry out pre-burning, take it out after cooling; transfer the pre-fired corundum crucible with samples into a large corundum crucible in the microwave oven, and fill the gap between the two crucibles with a 1:1 mass ratio of iron oxide and nickel oxide to absorb waves Material; 95N was introduced into the reaction chamber 2 +5%H 2 reducing gas, start the power of the microwave oven, control the power of the microwave oven to 1 kW, and burn for 6 hours; turn off the power of the microwave oven and the reducing gas, and cool naturally to room temperature to obtain the phosphor product. attached figure 2 For the obtained (Sr, ...

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Abstract

The present invention is microwave sintering process of RE luminophor material. RE gel powder prepared through atomizing process after being pre-sintered is sintered in reducing atmosphere inside a microwave oven to obtain the RE luminophor material. The RE gel powder includes RE aluminate, RE silicate and RE aluminosilicate system. The microwave radiation heating process has simultaneous material inside and outside heating, quick temperature raising, high crystallizing speed and small crystal grains, and is superior to available technology.

Description

【Technical field】 [0001] The invention relates to the technical field of luminescent materials, in particular to a microwave firing method for rare earth phosphor materials. 【Background technique】 [0002] In the applicant's published patents (CN1775905, CN1775904 and CN1786108), a method for producing xerogel powder by atomization of rare earth composite sol is described. [0003] The high-temperature electric furnace firing method is a traditional method for preparing rare earth luminescent materials. The main disadvantages are: (1) The fired product has large grains, high density, and high hardness, and ball milling is usually required; (2) The firing temperature is high and the reaction time is high. It takes a long time to cool the product, and the product often has a small amount of mesophase in addition to the main crystal phase; (5) Calcination at a higher temperature consumes more energy. The firing of rare earth phosphors in industrial tunnel kilns is another meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/77
Inventor 王达健
Owner 艾柯谷生态农业发展(河北)有限公司