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Preparation method of M3Si6O12N2: xRe system green fluorescent powder

An m3si6o12n2, green phosphor technology, applied in the field of luminescent materials, can solve the problems such as the lack of specific disclosure of the relevant performance of the microwave heating method, the immature preparation technology of violet LED chips, the lack of high-efficiency phosphors, etc., so as to shorten the production cycle and the holding time. Shortening, narrow particle size distribution effect

Inactive Publication Date: 2013-01-23
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The color rendering of white LEDs obtained by the third method is significantly improved, but high-efficiency phosphors are still relatively scarce, there are color reabsorption and ratio control problems between phosphors, and the preparation technology of violet LED chips is not yet mature, these factors lead to Near-ultraviolet conversion white light LEDs are difficult to obtain large-scale applications in the short term; while the second method has the advantages of the other two methods. The blue light is mixed with the red light and green light converted by the phosphor to generate white light, which has good color reproduction and meets the requirements of human vision. Therefore, high-performance red and green phosphors are a key factor
In addition, the Chinese patent application with the application number 201110152682.4 discloses a method for preparing nitride / oxynitride phosphors for white light LEDs by microwave heating method, but for this white light and backlight LEDs, M 3 Si 6 o 12 N 2 : The green phosphor of the xRe system, which does not specifically disclose the relevant properties when prepared by microwave heating method, etc.

Method used

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  • Preparation method of M3Si6O12N2: xRe system green fluorescent powder
  • Preparation method of M3Si6O12N2: xRe system green fluorescent powder
  • Preparation method of M3Si6O12N2: xRe system green fluorescent powder

Examples

Experimental program
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Effect test

Embodiment 1

[0036] m 3 Si 6 o 12 N 2 :xEu 2+ Phosphor powder, wherein M=Ba, the synthetic method of x=0.2 is as follows:

[0037] With the chemical formula Ba 3 Si 6 o 12 N 2 :xEu 2+ The stoichiometric ratio in (x=0.2) weighs an appropriate amount of BaCO 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 1250°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 resulting product is a gree...

Embodiment 2～7

[0040] Same as Example 1, Examples 2-7 are also M 3 Si 6 o 12 N 2 :xEu 2+ The synthetic method of fluorescent powder fluorescent powder, this method is basically identical with embodiment 1, difference is chemical formula M 3 Si 6 o 12 N2 :xEu 2+ The values ​​of M, x, M raw materials, synthesis temperature, and holding time in M ​​are different values, as shown in Table 1 below.

[0041] Table 1: Synthesis of M in Examples 2-6 3 i 6 o 12 N 2 :xEu 2+ Component content and process conditions of phosphor powder

[0042]

[0043] Fluorescence spectroscopy and particle size analysis were used to characterize the prepared powders. From the phase analysis results of the test, it can be seen that the powder consists of pure phase M 3 Si 6 o 12 N 2 Composition, and good crystallinity; powder particle size distribution range is narrow, regular shape, good particle dispersibility; luminescence characteristics and particle size are shown in Table 2 below.

[0044] Tab...

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Abstract

The invention discloses a preparation method of M3Si6O12N2: xRe system green fluorescent powder. According to the preparation method, M is one or the mixture of more than two of Ca, Sr and Ba; Re means a rare-earth element; and x is more than or equal to 0.2 mol% and less than or equal to 20mol%. The method comprises the steps as follows: weighing raw materials based on the stoichiometric ratio of various elements in the chemical formula of fluorescent powder; fully and uniformly mixing the raw materials; then placing the mixture into a sagger manufactured by a wave-transmitting material; positioning the sagger into a special microwave oven; adjusting the microwave power to control the temperature raise rate under a certain gas atmosphere; heating to reach the synthesizing temperature; and finally, cooling and simply grinding to obtain the system green fluorescent powder. Compared with traditional high-temperature solid phase method, the preparation method disclosed by the invention adopts microwave heating, therefore, the synthesizing temperature is reduced to 1000 to 1500 DEG C, moreover, the reaction time is reduced, and the production efficiency is improved; and the prepared green fluorescent powder has the advantages of fine grain size, high crystallizing performance, narrow range of size distribution, regular appearance and shape, high particle dispersing performance, and the like, and is specifically applied to white light and backlight LEDs (Light Emitting Diodes).

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, in particular to a M 3 Si 6 o 12 N 2 : The preparation method of xRe system green fluorescent powder is especially suitable for white light and backlight LED. Background technique [0002] White light LED (or semiconductor lighting) has the characteristics of green environmental protection, long life, high efficiency and energy saving, anti-harsh environment, simple structure, small size, light weight, fast response, low working voltage and good safety, so it is known as the successor The fourth-generation lighting electric light source after incandescent lamps, fluorescent lamps and energy-saving lamps, or called the 21st century green light source. [0003] White LEDs can be realized through a variety of methods, among which (1) the combination of blue LED chips and yellow phosphor powder is the earliest and most mature method. The luminous efficiency of the prepared white LED...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/59H01L33/50
CPCY02B20/181Y02B20/00
Inventor 王义飞黄庆胡春峰刘丽红李万元
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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