Silicon-based nitrogen oxide fluorescent powder as well as preparation method and application thereof

An oxynitride and phosphor technology is applied in the field of silicon-based oxynitride phosphors and their preparation, which can solve the problems of low cost, high quenching temperature and good system stability of green phosphors, and widen the spectral emission range. , The effect of high luminous intensity and high yield

Active Publication Date: 2017-02-22
HEBEI LIFU CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to provide a silicon-based oxynitride phosphor to solve the problem that the e

Method used

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  • Silicon-based nitrogen oxide fluorescent powder as well as preparation method and application thereof
  • Silicon-based nitrogen oxide fluorescent powder as well as preparation method and application thereof
  • Silicon-based nitrogen oxide fluorescent powder as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] According to Ba 1.95 Mg 0.05 SiO 4 :0.04Eu 2+ ,0.04Y 3+ The stoichiometric ratio of the carbonates or oxides of each element in the flux and the flux is taken by weighing the raw material BaCO 3 430.51g, MgO2.25g, SiO 2 67.21g, Eu 2 o 3 7.87g, Y 2 o 3 5.05g, CaCl 2 6.21g (5% of the molar number of Si), mix well, and after ball milling for 10h, put it in a corundum crucible, open the cover, place the crucible in a tube furnace, and put it in a 3:1 volume ratio of N 2 、H 2 In the mixed gas, the temperature was raised to 1350°C at a rate of 10°C / min, and then kept for 4 hours, then naturally cooled to room temperature, taken out and crushed, passed through a 200-mesh sieve, washed with alcohol, and dried to obtain the precursor Q required for secondary sintering.

[0057] Weigh 400g of the above precursor Q, according to Q (Si 3 N 4 ) 1 Weighing Si in the middle proportion 3 N 4 155.4g, flux SrF 2 5.55g, mixed evenly, after ball milling for 10h, place...

Embodiment 2

[0067] According to Sr 1.95 Mg 0.05 SiO 4 :0.04Eu 2+ ,0.04Y 3+ The stoichiometric ratio of the carbonates or oxides of each element in the flux and the flux is taken by weighing the raw material BaCO 3 411.29g, MgO2.88g, SiO 2 85.84g, Eu 2 o 3 10.06g, Y 2 o 3 6.45g, CaCl 2 7.93g (5% of the molar number of Si), mix well, and after ball milling for 10h, place in a corundum crucible, open the cover, place the crucible in a tube furnace, and place it in a 3:1 volume ratio of N 2 、H 2 In the mixed gas, the temperature was raised to 1350°C at a rate of 10°C / min, and then kept for 4 hours, then naturally cooled to room temperature, taken out and crushed, passed through a 200-mesh sieve, washed with alcohol, and dried to obtain the precursor Q required for secondary sintering.

[0068] Weigh 400g of the above precursor Q, according to Q (Si 3 N 4 ) 1 Weighing Si in the middle proportion 3 N4 220.38g, flux SrF 2 6.2g, mixed evenly, after ball milling for 10h, placed...

Embodiment 3～7

[0074] The proportioning of major ingredients is determined according to each general formula in table 4, and the preparation steps and process conditions are the same as in Example 2, wherein the source of Ge is GeO 2 .

[0075] Table 4:

[0076]

[0077] Compared with Example 2, the incorporation of Ge causes a certain degree of blue shift in the system, and a green phosphor of 530nm to 540nm is obtained. It is normal to decrease the luminous intensity by shifting, but when the Ge doping amount reaches 0.2, the luminous intensity of the system is only half of that of Example 2, which is far lower than the 530nm luminous intensity of the common corresponding silicate. Therefore, the Ge doping amount should not be too high high.

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Abstract

The invention discloses silicon-based nitrogen oxide fluorescent powder as well as a preparation method and application thereof. A general chemical formula of the fluorescent powder is Q.(Si<3>N<4>)<K>, wherein in the formula, k is more than 0.8 and less than 1.2. The fluorescent powder is synthesized through the following two steps: firstly synthesizing a precursor Q and then synthesizing the silicon-based nitrogen oxide fluorescent powder, wherein a general chemical formula of the precursor Q is M<x>(Si,A<2>)O<2+x>:yEu<2+>, zA<1><3+>; in the formula, M is at least one of Sr, Ba, Mg, Ca, Zn, Cu and Mn; A1 is at least one of Y, La, Sc and Er; A2 is not added or A2 is Ge; x is not less than 1.9 and not more than 2.1; y is not less than 0.005 and not more than 0.2; z is not less than 0.01 and not more than 0.2. The fluorescent powder provided by the invention can be effectively excited by 300nm-470nm wavelength to emit blue-green light or green-yellow light with peak wavelength of 490nm-560nm, has high quantum efficiency, narrow full width at half maximum (FWHM) and high thermal quenching temperature and can be matched with blue chips-ultraviolet chips to be applied to the field of white LED or display.

Description

technical field [0001] The invention relates to a fluorescent powder and its preparation method and application, in particular to a silicon-based nitrogen oxide fluorescent powder and its preparation method and application. Background technique [0002] Light-emitting diodes (LEDs) have many advantages such as energy saving, environmental protection, safety, multi-color, high light efficiency, long life, low driving voltage, and anti-vibration. At present, the mainstream white light LED uses InGaN blue light chips to excite YAG:Ce 3+ Phosphor powder produces yellow light complementary to blue light, which is then mixed to achieve. However, since YAG:Ce 3+ In phosphor, the spectral energy of red light accounts for about 8-15% of the total spectral energy, which is far lower than the proportion of yellow-green light. Therefore, the color rendering index of products manufactured by this method is low, generally around 70; and the color temperature is high , basically above 5...

Claims

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Application Information

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IPC IPC(8): C09K11/59C09K11/66H01L33/50
CPCC09K11/0883C09K11/7792C09K11/7793H01L33/502H01L2933/0041
Inventor 杨志平刘少鹏董秀芹赵金鑫
Owner HEBEI LIFU CHEM TECH
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