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Preparation method for fluorescent powder with structure similar to Si3N4 and prepared fluorescent powder

A fluorescent powder, -si3n4 technology, applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of harsh synthesis conditions, poor reactivity, residues, etc., to shorten the production cycle, meet the crystallinity and light efficiency, and improve the synthesis reaction speed effect

Active Publication Date: 2014-12-03
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But since Si 3 N 4 Has a strong covalent bond, low diffusion coefficient, and poor reactivity, so Si 3 N 4 The conditions for the synthesis of nitrides / nitrogen oxides as raw materials are often harsh
[0004] At present, the means of preparing nitride / oxynitride phosphors have evolved from the process of preparing ceramic materials, such as high-temperature and high-pressure nitriding, gas-phase reduction nitriding, carbothermal reduction nitriding (CRN) or self-propagating high-temperature synthesis (SHS ), etc.; where high-temperature, high-pressure nitriding and self-propagating high-temperature synthesis require high temperature (1700-2200°C), high pressure (5-10atm) and other conditions, while gas-phase reduction nitriding requires long-term high-temperature nitriding reduction, carbothermal reduction Nitriding is prone to carbon residues
In recent years, my country has carried out many researches on nitride / nitride phosphors, but due to the barriers of synthesis technology, the application pace of practical high-performance rare earth nitride / nitride phosphors is limited.

Method used

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  • Preparation method for fluorescent powder with structure similar to Si3N4 and prepared fluorescent powder
  • Preparation method for fluorescent powder with structure similar to Si3N4 and prepared fluorescent powder
  • Preparation method for fluorescent powder with structure similar to Si3N4 and prepared fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The Si-like prepared in this example 3 N 4 The chemical formula of structural phosphor is (Sr 0.999 / 3 Al 0.81 / 3 Si 4 / 3 ) 3 (N 6.8 / 4 ) 4 :0.001Eu 2+ . Its preparation method is: weigh an appropriate amount of Sr according to the stoichiometric ratio of each element in the chemical formula 3 N 2 、Si 3 N 4 , AlN, EuN as raw materials and grind and mix evenly, where Si 3 N 4 The raw material is made of α-Si 3 N 4 and β-Si 3 N 4 Composed of, and β-Si 3 N 4 and α-Si 3 N 4 The molar ratio is 0.005. The mixed raw materials were put into a crucible, and then kept at 1650° C. for 8 hours in a nitrogen atmosphere. After the reaction is completed, take out the product when the temperature drops below 100°C, and finally perform crushing, washing, drying and other treatments to obtain a Si-like 3 N 4 Structured Phosphors. The light color data such as the main peak position and relative luminous brightness of the phosphor powder are shown in Table 1.

Embodiment 2-6

[0030] The fluorescent powder preparation method of embodiment 2-6 is substantially the same as embodiment 1, and is (M a1 Al b1 Si cl ) 3 (N d1 ) 4 :x 1 Eu 2+ The preparation method of phosphor, the difference is the element composition in the chemical formula and the β-Si in the raw material 3 N 4 and α-Si 3 N 4 The molar ratio is shown in Table 1.

[0031] The light color data such as the main peak position and relative luminous brightness of the phosphor powders of these embodiments are shown in Table 1. Apply XRD, SEM and fluorescence spectrum to characterize embodiment 5 fluorescent powder, the result that obtains is respectively as follows figure 1 , figure 2 and image 3 shown. From figure 1 It can be seen that the prepared phosphor has a single phase (Sr 0.9 / 3 Al 1.2 / 3 Si 4 / 3 ) 3 (N 7.2 / 4 ) 4 :0.1Eu 2+ , and, from figure 2 It can be seen that the crystallinity of the phosphor powder is good, and the crystal morphology is clear and columnar. F...

Embodiment 7

[0033] The Si-like prepared in this example 3 N 4 The chemical formula of structural phosphor is (Sr 0.95 / 3 Ca 0.25 / 3 Al 1 / 3 Si 3.81 / 3 ) 3 (N 6.98 / 4 ) 4 :0.15Eu 2+ . Its preparation method is: weigh an appropriate amount of Ca according to the stoichiometric ratio of each element in the chemical formula 3 N 2 、Sr 3 N 2 、Si 3 N 4 , AlN, EuN as raw materials and grind and mix evenly, where Si 3 N 4 The raw material is made of α-Si 3 N 4 and β-Si 3 N 4 Composed of, and β-Si 3 N 4 and α-Si 3 N 4 The molar ratio is 0.5. The mixed raw materials were put into a crucible, and then kept at 1650° C. for 8 hours in a nitrogen atmosphere. After the reaction is completed, take out the product when the temperature drops below 100°C, and finally perform crushing, washing, drying and other treatments to obtain a Si-like 3 N 4 Structured Phosphors. The light color data such as the main peak position and relative luminous brightness of the phosphor powder are shown i...

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Abstract

The invention discloses a preparation method for a fluorescent powder with a structure similar to Si3N4 and the prepared fluorescent powder. The preparation method comprises: weighing raw materials according to a stoichiometric ratio of elements in the fluorescent powder chemical formula, fully mixing the raw materials, keeping warm and sintering at 1300-1850 DEG C under normal pressure for 5-20 h, and finally performing crushing, washing, drying and other processing operations on the sintered product, so as to obtain the fluorescent powder. In the raw materials, a Si source is composed of alpha-Si3N4 and beta-Si3N4. Compared with the prior art, the preparation method of the fluorescent powder is short in needed sintering time, and the fluorescent powder with the structure similar to Si3N4 prepared under normal pressure has the advantages of good crystallinity, high luminous efficiency and the like.

Description

technical field [0001] The invention belongs to the technical field of semiconductors, in particular to a Si-like 3 N 4 A method for preparing a structured phosphor and the phosphor produced therefrom. Background technique [0002] Compared with conventional light-emitting technologies such as incandescent lamps or fluorescent lamps, white light-emitting diodes (Light Emitting Diode, LED), as a new generation of green lighting products, have the advantages of low voltage, high luminous efficiency, low energy consumption, long life, no pollution, and small size. , fast response, low heat generation and high reliability, it has been successfully applied in the field of semiconductor lighting and backlight display, and it is a strategic emerging industry focused on development in my country. [0003] At this stage, phosphor plays a key role in white LED technology, and its performance determines key technical parameters such as luminous efficiency, color temperature, color ren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64C09K11/59
Inventor 周小芳庄卫东刘荣辉刘元红徐会兵何华强陈观通
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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