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A kind of preparation method of nitride/oxynitride fluorescent powder for white light LED

A technology of oxynitride and nitride, applied in the field of preparation of nitride/oxynitride phosphors for white light LEDs

Inactive Publication Date: 2011-11-30
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, for nitride / oxynitride phosphors, due to the limitation of high temperature and high pressure synthesis conditions, the traditional high temperature and pressure synthesis method is still used at present, and there is no related report on the use of microwave heating method.

Method used

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  • A kind of preparation method of nitride/oxynitride fluorescent powder for white light LED
  • A kind of preparation method of nitride/oxynitride fluorescent powder for white light LED
  • A kind of preparation method of nitride/oxynitride fluorescent powder for white light LED

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Ca~alpha~Si 12～(m+n) Al m+n o n N 16～n :xEu 2+ The synthesis method of phosphor powder is as follows:

[0052] with chemical formula M val+ m / val+ Si 12～(m+n) Al m+n o n N 16～n :xEu 2+ (wherein M=Ca, m=2, n=1, x=0.07) stoichiometric ratio takes an appropriate amount of Si 3 N 4 , AlN, Eu 2 o 3 , CaCO 3 as a raw material, and then place the raw material on the Si 3 N 4 Mix and grind in a mortar; put the ground material into a BN saggar, then put it in a microwave oven, and pass through the N 2 with H 2 The mixed gas, the H in the mixed gas 2 The mass percentage content is 5%; by adjusting the power, heat up to 1550°C at a heating rate of 40°C / min and a gas flow rate of 0.3L / min, and keep it at normal pressure for 2 hours; turn it off after the reaction is completed Microwave source, the reactants are naturally cooled to room temperature, after taking out, through Si 3 N 4 Brief grinding in a mortar gave the product as a yellow powder.

[0053] The ...

Embodiment 2～10

[0056] Same as Example 1, Examples 2-10 are also Ca~alpha~Si 12～(m+n) Al m+n o n N 16～n :xEu 2+ The synthetic method of fluorescent powder, this method is basically identical with embodiment 1, and difference is chemical formula M val+ m / val+ Si 12～ (m+n) Al m+n o n N 16～n :xEu 2+ The values ​​of M, m, n, and x in , as well as the synthesis temperature and holding time adopt different values, as shown in Table 1 below.

[0057] Table 1: Synthesis of alpha-SiAlON:Eu in Examples 2-10 2 Component content and process conditions of phosphor powder

[0058]

[0059]

[0060] XRD, fluorescence spectrum, particle size distribution and quantum efficiency were used to characterize the powders prepared in Examples 2-10 above. Phase analysis results are similar to figure 2 , From the phase analysis results of the test, it can be seen that the powder is composed of a single phase of alpha-SiAlON, and it can be seen from the XRD diffraction peak that the prepared powder...

Embodiment 11

[0064] MSi 2 o 2 N 2 :xEu 2+ (M=Sr, Ca, Ba, Mg) the synthetic method of fluorescent powder is as follows:

[0065] With chemical formula MSi 2 o 2 N 2 :xEu 2+ The stoichiometric ratio in (M=Sr, x=0.05) weighs an appropriate amount of SrCO 3 , SiO 2 、Si 3 N 4 and Eu 2 o 3 As a raw material, the raw material is then mixed and ground in an agate mortar; the ground raw material is charged into Al 2 o 3 Sagger, place the sagger in Al 2 o 3 In the heat preservation barrel, fill the insulation cotton between the sagger and the heat preservation barrel, and place SiC auxiliary heating material on the outer wall of the sagger; At a gas flow rate of 0.3L / min, heat to 1500°C under normal pressure and keep it warm for 2 hours; after the reaction is completed, turn off the microwave source, and the reactant is naturally cooled to room temperature with the furnace, and the synthesized phosphor is simply ground through an agate mortar , the obtained product is a yellow-green...

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Abstract

Provided is a method for preparing a nitride / oxynitride fluorescent powder used by a white LED. The raw material is weighted according to the chemometry of each element in the chemical formula of a nitride / oxynitride fluorescent powder and loaded into a sagger made of a wave-transparent material after being mixed uniformly, then the sagger is placed into a professional microwave oven, in a fixed gas atmosphere, and the fluorescent powder is obtained by adjusting the microwave power to control the warming rate, heating to the resultant temperature, and finally cooling and grinding. As compared to methods in the prior art, the method is performed under normal pressure, reducing the resultant temperature, shortening the production period, and greatly reducing the production costs; and the fluorescent powder obtained has good crystallinity, fine grain size, a narrow granularity distribution range, good grain dispersibility, and a regular shape.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a method for preparing a nitride / oxynitride fluorescent powder for white light LEDs. Background technique [0002] At present, the total electricity consumption of lighting in the world accounts for about 40% of the total electricity consumption in the world. Seeking new lighting sources with both power saving and environmental protection concepts has become an urgent problem to be solved by governments and scientific research circles. Compared with traditional incandescent lamps, fluorescent lamps and high-intensity gas discharge lamps, white LEDs, which realize photoelectric conversion through semiconductor light-emitting diodes, not only have the characteristics of high luminous efficiency, long life, low energy consumption and no pollution to the environment, but also have high brightness, With the advantages of small size, fast response, low heat ge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64C09K11/59
CPCY02B20/181C09K11/0883C09K11/7792H05B33/14C09K11/7734C09K11/64C09K11/59H01L2933/0041C09K11/77347C09K11/77348
Inventor 黄庆刘丽红周小兵
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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