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Red Nitrogen oxide fluorescent powder and preparation method thereof

A technology of nitrogen oxides and phosphors, which is applied in the field of phosphors and its preparation, can solve the problems of unfavorable mass production, high price, and easy oxidation, and achieve excellent thermal quenching resistance, low cost, and simple preparation process Effect

Inactive Publication Date: 2014-04-02
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, M 2 Si 5 N 8 :Eu 2+ (M=Ca, Sr, Ba) and CaAlSiN 3 :Eu 2+ The preparation of such red phosphors usually requires the use of high-purity nitrides (such as Ca 3 N 2 , SrN x 、BaN x 、EuN x etc.), or high-purity metals (Ca, Al, Si, Eu, etc.) There is even an explosion hazard, which is very unfavorable for mass production (Y.Q.Li et al.Luminescence properties of red-emitting Sr 2 Si 5 N 8 :Eu 2+ (M=Ca, Sr, Ba) LED conversion phosphors. J. Alloys Compd., 2006, 417: 273-279. K Uheda et al. Luminescence properties of a red phosphor CaAlSiN 3 :Eu 2+ for white light emitting diodes. Electrochem. Solid-state Lett., 2006, 9(4): H22-H25)

Method used

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  • Red Nitrogen oxide fluorescent powder and preparation method thereof
  • Red Nitrogen oxide fluorescent powder and preparation method thereof
  • Red Nitrogen oxide fluorescent powder and preparation method thereof

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preparation example Construction

[0035] The invention relates to a red nitrogen oxide fluorescent powder and a preparation method thereof. The phosphor is based on α-Si 3 N 4 The nitride or oxynitride crystal of the crystal structure is formed by solid-dissolving Mn, and the fluorescence with a peak in the wavelength range of 600-750nm will be emitted by irradiating an ultraviolet or visible light excitation source.

[0036] The general chemical formula of the fluorescent powder of the present invention is M (m-2x) / v mn x Si 12-(m+n) al (m+n) o n N 16-n , where M is the metal ion (M=Li, Ca, Mg or Y), v is the valence of the metal M ion, 0<x<1, 0<m≤2(v+x), 0≤n≤2(v +x).

[0037] The characteristics of the nitrogen oxide phosphor powder provided by the present invention mainly lie in:

[0038] (1) Oxynitride phosphor, contained in α-Si 3 N 4 The crystal of the crystal structure has a solid solution of Mn nitride or nitrogen oxide crystal, and the fluorescence with a peak wavelength in the wavelength r...

Embodiment 1-7

[0053] The raw materials used in each embodiment are as follows:

[0054] Si 3 N 4 Powder: α phase content ≥ 92%, O content 0.98%, Fe content ≤ 100ppm, median grain size d 50 =0.32μm

[0055] AlN powder: N content ≥ 32%, Fe content ≤ 100ppm

[0056] CaCO 3 Powder: purity ≥ 99.9%, Fe content ≤ 100ppm

[0057] MnCO 3 Powder: purity ≥ 99.9%, Fe content ≤ 100ppm

[0058] Nitrogen (N 2 ): Purity ≥ 99.9%.

[0059] Formulation design: according to the chemical formula Ca 0.80-x mn x Si 9.6 al 2.4 o 0.8 N 15.2 (Ca-α-SiAlON:Mn 2+ ) designed 7 formulations (x=0.02, 0.05, 0.10, 0.12, 0.15, 0.20, 0.50), and any formulation was processed according to the following methods and steps.

[0060] Weighing: Using the above powder as the starting material, weigh various powder materials in strict accordance with the above stoichiometric ratio.

[0061] Mixing: In a high-purity silicon nitride ball mill tank, use high-purity silicon nitride balls and anhydrous ethanol solvent to w...

Embodiment 8-14

[0076] Use the fluorescent powder prepared in Examples 1-7 to carry out follow-up heat treatment: (1) vacuum the inside of the firing chamber to 10 by a vacuum system -2 Above Pa; (2) Heating from room temperature to 1000°C at a heating rate of 10°C / min; (3) Introducing high-purity nitrogen with a purity of 99.9% at 1000°C to make the pressure in the sintering furnace chamber reach the range of 0.80-0.85MPa; (4) Under the condition of nitrogen pressure of 0.80-0.85MPa (when the internal pressure of the furnace chamber is lower than 0.80MPa, the equipment will automatically replenish the gas, and when the furnace chamber pressure reaches 0.85MPa, the equipment will automatically deflate), at a rate of 10°C / min The heating rate is from 1000°C to 1600°C; (5) Under the condition of nitrogen pressure of 0.80-0.85MPa, heat preservation treatment at 1600°C for 10h; (6) After heat preservation treatment at 1600°C for 10h, naturally cool to room temperature.

[0077] Grinding and crush...

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Abstract

The invention provides new red nitrogen oxide fluorescent powder and a preparation method of the red nitrogen oxide fluorescent powder. The fluorescent powder provided by the invention comprises crystallines in which nitrides or nitrogen oxides of Mn are solid dissolved in crystals with a alpha-Si3N4 crystal structure, the crystals with the alpha-Si3N4 crystal structure comprises alpha-Sialon, and the fluorescent powder can emit fluorescence through irradiating an excitation source, wherein the fluorescence has a peak in the wavelength range of 600-750nm. The fluorescent powder provided by the invention has excellent thermal quenching resisting property, and has important application prospect in the fields of white LED (light emitting diode) lighting, field emission display (FED), plasma display panel (PDP) and the like.

Description

technical field [0001] The present invention relates to a kind of α-type Si 3 N 4 Phosphor powder with crystal structure and its preparation method. The phosphor is based on α-Si 3 N 4 The nitride or oxynitride crystal of the crystal structure is formed by solid-dissolving Mn, and the fluorescence with a peak in the wavelength range of 600-750nm will be emitted by irradiating an ultraviolet or visible light excitation source. Background technique [0002] Since the 1990s, with the advancement of light-emitting diode (Light-Emitting Diode, LED) technology, especially the development of white LEDs, LEDs have been used in special light source applications (such as large-screen displays, indicator lights, landscape lighting, backlights, etc.) sources, etc.) gradually into general lighting. Due to the comprehensive advantages of LEDs such as high brightness, high color rendering index, energy saving, environmental protection, long life, small size, fast response, high reliab...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/80C09K11/64
CPCY02B20/181Y02B20/00
Inventor 刘学建张玉强黄政仁
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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