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A kind of preparation method of silicon-based oxynitride fluorescent powder

An oxynitride and phosphor technology is applied in the field of preparation of silicon-based oxynitride phosphors, which can solve the problems of harsh equipment and synthesis conditions, poor performance control, unfavorable mass production, etc. Excellent decay performance and high quantum efficiency

Active Publication Date: 2016-01-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of silicon-based oxynitride phosphor by conventional sintering method is relatively harsh on raw materials, equipment and synthesis conditions.
And there are too many raw material components, which makes the performance of the final product difficult to control and is not conducive to mass production

Method used

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  • A kind of preparation method of silicon-based oxynitride fluorescent powder
  • A kind of preparation method of silicon-based oxynitride fluorescent powder
  • A kind of preparation method of silicon-based oxynitride fluorescent powder

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Polycarbosilane and europium acetylacetonate are used as raw materials, and the mass ratio of the two is 5:1. After the two raw materials were fully mixed and ground for 0.5h, they were put into a three-necked glass bottle, and after being fully pumped with nitrogen for three times, under the protection of nitrogen atmosphere, the temperature was raised to 320°C at a rate of 1°C / min, and kept for 6h. After the synthesized product was fully mixed and ground for 0.5h, it was placed in an alumina crucible, gas exchanged three times, and the temperature was raised to 800°C at a rate of 1°C / min under an ammonia atmosphere, and kept for 1h; The temperature was raised to 1350°C at a speed of 1 / min, and the temperature was kept for 3 hours. The obtained product can be obtained phosphor powder after thorough grinding. Its XRD diagram and emission spectrum diagram refer to figure 1 and figure 2 .

Embodiment 2

[0028] Polycarbosilane, europium acetylacetonate and magnesium acetylacetonate are used as raw materials, and the mass ratio is 20:1:0.2. The three raw materials were thoroughly mixed and ground for 0.5 h, put into a three-necked glass bottle, and under the protection of a nitrogen atmosphere, the temperature was raised to 360 °C at a rate of 1 °C / min, and kept for 6 h. After the synthesized product was fully mixed and ground for 0.5h, it was placed in an alumina crucible, gas exchanged three times, and the temperature was raised to 700°C at a rate of 1°C / min under an ammonia atmosphere, and kept for 3h; The temperature was raised to 1450°C at a speed of 1 / min, and the temperature was kept for 3 hours. The obtained product can be obtained phosphor powder after thorough grinding. For its emission spectrum see image 3 .

Embodiment 3

[0030] Polycarbosilane, europium acetylacetonate and magnesium acetylacetonate are used as raw materials, and the mass ratio is 40:1:0.5. After the three raw materials were fully mixed and ground for 0.5h, they were put into a three-necked glass bottle, and under the protection of nitrogen atmosphere, the temperature was raised to 400°C at a rate of 1°C / min, and kept for 6h. The synthesized product was mixed and ground for 0.5h, then put into an alumina crucible, gas exchanged three times, heated to 900°C at a rate of 1°C / min under an ammonia atmosphere, and kept for 1h; The temperature was raised to 1550°C at a speed of 1 min, and the temperature was kept for 3 hours. The obtained product can be obtained phosphor powder after thorough grinding. For its emission spectrum see Figure 4 .

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Abstract

The invention discloses a preparation method of silicon-based oxynitride fluorescent powder, and relates to a preparation method of fluorescent powder. The method comprises the following steps: mixing precursor raw materials: polycarbosilane, europium acetylacetone and acetylacetone; filling in a reaction container after grinding; after placement by nitrogen, under the protection of nitrogen atmosphere, and after heating reaction, naturally cooling to room temperature; grinding the obtained product, and sintering and grinding to obtain the silicon-based oxynitride fluorescent powder. By replacing the raw materials such as pure metals and metal nitrides which are expensive in price and unstable in chemical property in the existing process of synthesizing the nitride fluorescent powder by substances stable in chemical property, the whole preparation process is simple and feasible. The raw materials required are less in variety, and products with different performances can be prepared by adopting different raw material proportions and matching a proper process. The preparation method is simple in requirement on equipment. The light emitting material is europium-activated nitride which is high in quantum efficiency, stable in physical and chemical properties and excellent antiaging performance. The excitation wavelength of the light material is wide, and the powder is suitable for excitation of light sources in various bands.

Description

technical field [0001] The invention relates to a method for preparing fluorescent powder, in particular to a method for preparing silicon-based oxynitride fluorescent powder. Background technique [0002] With the advancement of LED-related technologies, white LEDs have made great progress in terms of luminous efficiency, service life, and cost reduction. At present, the phosphors used generally have disadvantages such as low effective conversion efficiency or poor color rendering, while red and green phosphors with high conversion efficiency are mostly sulfide systems, which have poor luminescence stability and large light attenuation. Therefore, it is imminent to develop phosphors for white LEDs with high efficiency and low light attenuation. [0003] Nitride phosphor has unique excitation spectrum (excitation range covers ultraviolet, near ultraviolet, blue light and even green light) and excellent luminescence characteristics (emission of green, yellow, red light, smal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/59
Inventor 龚朝阳李泉张颖程璇涂惠彬
Owner XIAMEN UNIV