High-temperature microwave preparation method of red rare earth fluorescent material

A rare earth fluorescent material and microwave technology, applied in the direction of luminescent materials, chemical instruments and methods, sustainable manufacturing/processing, etc., can solve the problems of high firing temperature, high calcining energy consumption, high hardness, etc., achieve simple process, overcome The effect of sublimation of raw material components

Inactive Publication Date: 2013-07-10
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-temperature electric furnace firing method is a traditional method for preparing rare earth fluorescent 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 long. It also takes a considerable amount of time to cool the product. In addition to the main crystal phase, the product often has a small amount of intermediate phase; 3) Calcination at higher temperatures consumes more energy
The above-mentioned burning method lacks universal adaptability in the reduction method

Method used

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  • High-temperature microwave preparation method of red rare earth fluorescent material
  • High-temperature microwave preparation method of red rare earth fluorescent material
  • High-temperature microwave preparation method of red rare earth fluorescent material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A high-temperature microwave preparation method of a red rare earth fluorescent material, the steps are as follows:

[0019] 1) Weigh 4.1852g CaSO 4 , 2.8683gS, 0.0316gEu 2 o 3 , 0.0072g C and 0.0709gNH 4 Cl mixed and ground fully and then dried to obtain the mixture;

[0020] 2) Put half of the above mixture into corundum crucible A, put crucible A into crucible B, then add activated carbon powder whose filling height accounts for 30% of the net height of the interlayer into the interlayer of crucible A and B, and seal crucible B with a cover;

[0021] 3) Put the crucibles A and B as a whole into an industrial high-temperature microwave oven, and burn them at 1200°C for 1 hour. After the mixture is cooled, take out the mixture and grind it thoroughly;

[0022] 4) Then put the mixture into the crucible C, put the crucible C into an industrial high-temperature microwave oven, at 2.45 GHz, power 1.5 kW, pass in nitrogen-hydrogen mixed gas, and the H in the mixed gas ...

Embodiment 2

[0025] A high-temperature microwave preparation method of a red rare earth fluorescent material, the steps are as follows:

[0026] 1) Weigh 4.1852g CaSO 4 , 2.8683gS, 0.0316gEu 2 o 3 , 0.0072g C and 0.0709gNH 4 Cl mixed and ground fully and then dried to obtain the mixture;

[0027] 2) Put half of the above mixture into corundum crucible A, put crucible A into crucible B, then add activated carbon powder whose filling height accounts for 35% of the net height of the interlayer into the interlayer of crucible A and B, and seal crucible B with a cover;

[0028] 3) Put the crucibles A and B as a whole into an industrial high-temperature microwave oven, and burn them at 1100°C for 1 hour. After the mixture is cooled, take out the mixture and grind it thoroughly;

[0029] 4) Then put the mixture into the crucible C, put the crucible C into an industrial high-temperature microwave oven, at 2.45 GHz, power 1.5 kW, pass in nitrogen-hydrogen mixed gas, and the H in the mixed gas ...

Embodiment 3

[0032] A high-temperature microwave preparation method of a red rare earth fluorescent material, the steps are as follows:

[0033] 1) Weigh 4.1852g CaSO 4 , 2.8683gS, 0.0316gEu 2 o 3 , 0.0072g C and 0.0709gNH 4 Cl mixed and ground fully and then dried to obtain the mixture;

[0034] 2) Put half of the above mixture into corundum crucible A, put crucible A into crucible B, then add activated carbon powder whose filling height accounts for 40% of the net height of the interlayer into the interlayer of crucible A and B, and seal crucible B with a cover;

[0035] 3) Put the crucibles A and B as a whole into an industrial high-temperature microwave oven, and burn them at 1000°C for 1 hour. After the mixture is cooled, take out the mixture and grind it thoroughly;

[0036] 4) Then put the mixture into the crucible C, put the crucible C into an industrial high-temperature microwave oven, at 2.45 GHz, power 1.5 kW, pass in nitrogen-hydrogen mixed gas, and the H in the mixed gas ...

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PUM

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Abstract

The invention discloses a high-temperature microwave preparation method of a red rare earth fluorescent material. The red rare earth fluorescent material is prepared by using a two-step high-temperature microwave firing method, wherein in the first step, a matrix is formed by performing microwave firing; and in the second step, rare earth atoms are reduced by performing microwave firing. The method comprises the following steps of: mixing and fully grinding CaSO4, S, Eu2O3, C and a cosolvent NH4C1 and drying; putting the obtained mixture into an inner crucible sleeved into a corundum crucible; filling active carbon powder into an interlayer; putting into an industrial high-temperature microwave oven to fire under an air atmosphere; cooling and fully grinding; turning into another corundum crucible; and putting into the industrial high-temperature microwave oven to secondarily fire in nitrogen-hydrogen mixed gas to prepare the red rare earth fluorescent material. The high-temperature microwave preparation method has the advantages that based on the high-temperature microwave air firing, the matrix is formed by using a quickly-heating characteristic so as to overcome the defect of sublimation of raw material components of a sulfur-containing red rare earth fluorescent material. The method has the characteristics of energy-saving, quickness and effectiveness, simple process and puffed product particles, and can be directly applied to industrial production.

Description

【Technical field】 [0001] The invention belongs to the technical field of rare earth fluorescent materials, in particular to a high-temperature microwave preparation method of red rare earth fluorescent materials. 【Background technique】 [0002] The preparation of inorganic solid materials is one of the main research fields of material chemistry. Exploring new synthesis methods is a hot spot in this field. The purpose is to obtain new materials, new properties of materials, and synthesis methods that can be faster in time, In terms of energy, it saves energy, finally obtains a product with high purity and avoids the formation of various by-products in the reaction process as much as possible. The high-temperature electric furnace firing method is a traditional method for preparing rare earth fluorescent 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/56
CPCY02P20/10
Inventor 王达健马健王延泽陆启飞孙亮孙运杰董晓菲王芳
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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