Silicon nitride nanorod fluorescent powder and preparation method and application thereof

A technology of nanorods and phosphors, applied in nano optics, chemical instruments and methods, nanotechnology, etc., can solve problems such as high temperatures above 2000 °C, blue luminous properties, lack of trivalent states, etc., to achieve production Low cost, good economic and social benefits, and the effect of saving process steps and costs

Pending Publication Date: 2021-11-12
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of these compounds have complex structures, almost all of which are ternary, quaternary or even quinary compounds. The requirements for the types of raw materials are also various, which is not conducive to large-scale synthesis.
For example, the existing α-SiAlON for white LED: Eu 2+ Yellow phosphor, which introduces many types of atoms, and the synthesis temperature is too high, must reach above 2000 ° C; there is also a La 4-x Ca(SiO 4 ) 3 O:xCe 3+ , x=0.001~0.10 Yellow phosphor, although the synthesis method is straightforward and simple, but there are many types of raw ma...

Method used

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  • Silicon nitride nanorod fluorescent powder and preparation method and application thereof
  • Silicon nitride nanorod fluorescent powder and preparation method and application thereof
  • Silicon nitride nanorod fluorescent powder and preparation method and application thereof

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preparation example Construction

[0054] A method for preparing rare earth europium-doped silicon nitride nanorod fluorescent powder using crystalline silicon waste in the present invention comprises the following steps:

[0055] S1. Wash and dry the crystalline silicon waste and grind it into silicon powder, mix the silicon powder and the Eu source at a mass ratio of 1:(0.2-0.96) and grind it into a mixture powder of 50-400 meshes;

[0056] Preferably, the source of Eu is europium nitrate or europium acetate.

[0057] Preferably, the waste crystalline silicon is leftover material of monocrystalline silicon or polycrystalline silicon or waste materials of used crystalline silicon solar cells.

[0058] S2. Put the mixture powder ground in step S1 into a crucible, and then put the crucible into a high-temperature tube furnace;

[0059] S3, passing an inert gas into the high-temperature tube furnace, and performing sintering treatment at normal temperature and pressure;

[0060] Preferably, the inert gas is hig...

Embodiment 1

[0068] Clean and dry the leftovers of monocrystalline silicon, grind them into 50-mesh powder, mix the ground silicon powder and europium nitrate at a mass ratio of 1:0.48; then put them into a ceramic boat and place them in a high-temperature tube furnace. Feed high-purity nitrogen into the high-temperature tube furnace and turn on the high-temperature tube furnace. The flow rate of nitrogen is 30 sccm. The heating curve of the sample is first to 1000°C at a rate of 10°C / min, then to 1300°C at a rate of 4°C / min, and finally to 1440°C at a rate of 2°C / min. Insulate at this temperature for 3 hours, cool to room temperature after the reaction is over, and take out the sample to obtain silicon nitride yellow phosphor Si 3 N 4 : Eu.

[0069] figure 1 Given the obtained Si 3 N 4 : Scanning electron micrograph (SEM) of the Eu phosphor nanomaterial, it can be seen from the figure that the morphology of the nanomaterial is rod-shaped, and the diameter of the rod-shaped structure ...

Embodiment 2

[0071] Wash and dry the scraps of monocrystalline silicon, and grind them into 100-mesh powder. The ground silicon powder is mixed with europium nitrate at a mass ratio of 1:0.6; then put into a ceramic boat and placed in a high-temperature tube furnace. Feed high-purity nitrogen into the high-temperature tube furnace and turn on the high-temperature tube furnace. The flow rate of nitrogen is 100 sccm. The heating curve of the sample is first to 1000°C at a rate of 10°C / min, then to 1300°C at a rate of 4°C / min, and finally to 1500°C at a rate of 2°C / min. Insulate at this temperature for 2 hours, cool to room temperature after the reaction is over, and take out the sample to obtain silicon nitride yellow phosphor Si 3 N 4 : Eu.

[0072] figure 2 It is the emission spectrum diagram of the material under the excitation of 365nm ultraviolet light. The central position of the luminescence is 572 nanometers, and the half-minute width is about 95 nanometers. It is a phosphor wit...

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Abstract

The invention discloses silicon nitride nanorod fluorescent powder and a preparation method and application thereof. The preparation method comprises the steps that crystalline silicon waste is ground into silicon powder, Si powder and a europium source are weighed according to the proportion and fully mixed and ground, the ground mixture powder is put into a crucible and put into a high-temperature tube furnace, inert gas is introduced into the high-temperature tube furnace, and heated to a specified temperature at a certain heating rate, heat preservation is performed for a period of time, cooled to room temperature after heat preservation is finished, and ground to obtain the nitride yellow fluorescent powder. The substrate of the related fluorescent powder material is silicon nitride, the synthesis process is simple, waste is turned into wealth, an additional vacuum system is not needed, Eu < 2 + >/Eu < 3 + > coexistence can be realized, and the luminescence spectrum can be expanded and subjected to red shift. In addition, the obtained fluorescent powder is good in chemical stability, low in thermal quenching and high in luminous intensity, and can meet the requirements of fluorescent powder for high-power LEDs and the requirements of industrial production. (The attached drawing of the abstract is a composite spectrum and CIE drawing of the product and a blue light chip).

Description

technical field [0001] The invention belongs to the technical field of nanomaterials and luminescent powder preparation, and in particular relates to a silicon nitride nanorod fluorescent powder and a preparation method and application thereof. Background technique [0002] Due to its low energy consumption and high efficiency, white light-emitting diodes (LEDs) have developed rapidly and are gradually replacing traditional incandescent and fluorescent lamps, becoming a priority industry for national lighting projects. At present, there are three main methods to realize white LED: [0003] 1. Simultaneously excite red, green and blue phosphors with ultraviolet chips; [0004] 2. Direct combination of red, green and blue light-emitting chips; [0005] 3. Use the blue light chip to excite the yellow phosphor. [0006] The current mainstream commercial white LED is mainly the third implementation. Therefore, it is of great significance for the synthesis of yellow-emitting p...

Claims

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Application Information

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IPC IPC(8): C09K11/59B82Y20/00B82Y40/00H01L33/50
CPCC09K11/7734C09K11/0883B82Y20/00B82Y40/00H01L33/502Y02B20/00
Inventor 葛万银陆晨辉徐美美张盼锋张伟
Owner SHAANXI UNIV OF SCI & TECH
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