Preparation method of red fluorescence material

A technology of red fluorescent and powder materials, which is applied in the field of preparation of red fluorescent materials, can solve the problems of complex preparation process of luminescent materials, moisture absorption and deliquescence, oxidation reaction, lack of physical and chemical properties, etc., and achieve excellent luminescent performance, low cost, physical and chemical properties stable effect

Inactive Publication Date: 2014-03-26
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few international and domestic research reports on the preparation methods of nitride phosphors.
The traditional method mainly uses a variety of nitrides, sulfides, oxides, various salts and other raw materials to sinter in solid phase at high temperature. Due to the lack of good physical and chemical properties of the raw materials in the air, this method is difficult to purify, difficult to Crushing and grinding, moisture absorption and deliquescence, oxidation reaction, decomposition, corrosion of containers and equipment, etc., and due to these reasons, the preparation process of luminescent materials is complicated, difficult to operate, high cost, unreliable quality and other shortcomings
At present, there is no report on the preparation of luminescent materials by using alloy materials composed of Al, Si, Ca, Sr, Eu, etc.

Method used

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  • Preparation method of red fluorescence material
  • Preparation method of red fluorescence material
  • Preparation method of red fluorescence material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Select the dosing point X = 0.03, the molar ratio is 1:1 CaAl alloy with a purity of not less than 99.5%, Si 3 N 4 Powder, AlN and Eu 2 o 3 According to the molar ratio of 582:200:18:9, put it in a mortar, use absolute ethanol as the dispersion medium, fully grind until uniform, dry, and press into tablets; then load it in a graphite furnace, under 2 atmospheres of N 2 Under the protection of the atmosphere, sinter at a low temperature of 1100 ° C for 4 hours, and then in 4 atmospheres of N 2 Under the protection of the atmosphere, it was sintered at a high temperature of 1800°C for 10 hours and then cooled with the furnace. The prepared red fluorescent material has an excitation wavelength of 469nm and an emission wavelength of 620nm. Its excitation and emission spectra are figure 1 , 2 shown.

Embodiment 2

[0030] Select the dosing point X=0.03, the CaSi alloy with a molar ratio of 1:1 and a purity not lower than 99.5%, Si 3 N 4 Powder, AlN and Eu 2 o 3 According to the molar ratio of 194:2:200:3, put it in a mortar, use absolute ethanol as the dispersion medium, fully grind until uniform, dry, and press into tablets; then load it in a graphite furnace, under 1 atmosphere of N 2 Under the protection of the atmosphere, sinter at a low temperature of 1200 ° C for 3 hours, and then in 4 atmospheres of N 2 Under the protection of the atmosphere, it was sintered at a high temperature of 1700°C for 5 hours and then cooled with the furnace. The prepared red fluorescent material has an excitation wavelength of 469nm and an emission wavelength of 648nm. Its excitation and emission spectra are as image 3 , 4 shown.

Embodiment 3

[0032] Select the batching point X=0.03, mix the CaAl alloy with a molar ratio of 1:1 and the purity not less than 99.5%, Si powder, AlN and SiEu alloy with a molar ratio of 1:1, and the molar ratio is 97:97:3:3 , placed in a mortar, using absolute ethanol as the dispersion medium, fully ground until uniform, dried, and pressed into tablets; then loaded in a graphite furnace, under 2 atmospheres of N 2 Under the protection of the atmosphere, sinter at a low temperature of 1100 ° C for 3 hours, and then in 4 atmospheres of N 2 Under the protection of the atmosphere, it was sintered at a high temperature of 1500°C for 4 hours and then cooled with the furnace. The prepared red fluorescent material has an excitation wavelength of 469nm and an emission wavelength of 628nm. Its excitation and emission spectra are as Figure 5 shown.

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Abstract

The invention belongs to the technical field of luminescent materials, in particular to a preparation method of a red fluorescence material. The method comprises the following steps: grinding binary or multicomponent alloy material of MAI into powder, wherein M is Si, Ca, Sr or Eu; mixing the nano-powder, powder of AIN and luminescence centre powder according to the molar ratio of 1-X:1 / 3:X:X, wherein X is more than 0 and less than 1; drying after mixing the above powder fully and tabletting for later use; loading the tablets into a graphite furnace, under the protection of N2 of 1-10 barometric pressure, presintering for 1-5 hours at the temperature of 1,000-1,200 DEG C, and sintering for 1-10 hours at the temperature of 1,500-1,800 DEG C; and then cooling the obtained product along with the furnace to obtain the red fluorescence material taking Eu2+ as a centre of luminescence. The preparation method has simple process, is easy to operate, and has excellent red luminous performance and chemical stability. The preparation raw materials of the method are the binary or multicomponent alloy materials with stable physicochemical property in the air.

Description

technical field [0001] The invention relates to the technical field of luminescent materials, in particular to a preparation method of red fluorescent materials. Background technique [0002] So far, a variety of luminescent materials have appeared and played an important role in various fields of society. But most of them are based on oxides, sulfides or oxysulfides, and a small amount of transition metal ions or rare earth ions are doped in these substrates as luminescent centers. The chemical stability of these compounds is poor, especially after combining the luminous efficiency and temperature quenching characteristics, there are not many practical materials. With the development of society, it has become more and more difficult for them to adapt to the material requirements of white light diode lighting and modern plasma and field emission display technology. [0003] when Ce 3+ or Eu 2+ When used as an activator, its absorption and emission bands are determined by...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/80
Inventor 刘泉林杨建军周天亮张贺边柳
Owner UNIV OF SCI & TECH BEIJING
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