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A β-sialon:eu 2+ Green fluorescent powder and its synthesis method

A green phosphor and phosphor technology, applied in the field of phosphors, can solve the problems affecting the brightness, light efficiency, uneven particle morphology of phosphors, complex overall process, etc., and achieve improved operability, particle uniformity, and simple process. Effect

Active Publication Date: 2017-09-19
HEBEI LIFU CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

European patents EP2570400A1 and EP2662430A1 provide a method for preparing β-SiAlON:Eu 2+ The process of phosphor powder, through heat treatment, strong acid (hydrofluoric acid plus nitric acid) acid treatment and other processes, the final sample particles obtained have poor uniformity, short particle size, particle diameter D50=5-6μm, and the overall process is complicated and the process is long. The operation is dangerous, the energy consumption is high, and the production cost is high
[0007] As can be seen from the above documents, the existing β-SiAlON:Eu 2+ In the solid-phase sintering method of green phosphor powder, the particle diameter of the product obtained by low-temperature sintering is less than 1 μm, and the particle shape is uneven, which seriously affects the brightness and light efficiency of the phosphor powder; while the preparation method introduced in European patent EP2570400A1 can obtain a little Coarse β-SiAlON:Eu 2+ Green fluorescent powder, particle diameter D50=5~6μm, but the overall process is complicated, the process is long, the operation is dangerous, the energy consumption is high, and the production cost is high

Method used

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  • A β-sialon:eu <sup>2+</sup> Green fluorescent powder and its synthesis method
  • A β-sialon:eu <sup>2+</sup> Green fluorescent powder and its synthesis method
  • A β-sialon:eu <sup>2+</sup> Green fluorescent powder and its synthesis method

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Example 1: β-SiAlON:Eu 2+ Preparation of phosphor

[0041] (1) According to the general formula Eu 0.011 Si 4.8 Al 0.21 O 0.067 N 6.573 Calculate the stoichiometric ratio of the elements in the 3 N 4 (Oxygen content 2 O 3 Powder (5N grade), Al 2 O 3 (4N grade)), then weigh and add flux (LiCl) to obtain the mixture:

[0042] α-Si 3 N 4 , AlN, Eu 2 O 3 , Al 2 O 3 Weigh with LiCl in proportions of 93.8wt%, 3.6wt%, 0.8wt%, 0.6wt%, 1.2wt%;

[0043] Where ɑ-Si 3 N 4 , AlN and Eu 2 O 3 Need to be in the glove box N 2 Weighing in a protected environment (H 2 O content ≤1ppm, O 2 Content≤1ppm);

[0044] (2) Take the α-Si 3 N 4 , AlN, Eu 2 O 3 , Al 2 O 3 Put LiCl in a ball mill mixer, dry blend for 0.5h, and then pass through a 100 mesh sieve;

[0045] After sieving, place it in a BN crucible, then put it in a high-temperature air pressure sintering furnace, first vacuum to 0.07Pa, and then charge N 2 Gas to 0.8MPa, and then start to heat up:

[0046] Stage 1: First, increase the temperatu...

Embodiment 2-20

[0051] Change the type of flux (see Table 1 for details), and other process conditions are the same as in Example 1.

Embodiment 21-26

[0053] The raw material ratio was changed to prepare phosphors with different elemental compositions (see Table 2 for details), and the other process conditions were the same as in Example 17.

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Abstract

The invention provides beta-SiAlON: Eu2 + green fluorescent powder. The chemical general formula of the green fluorescent powder is EuxSiaAlbOcNd, wherein the x is greater than or equal to 0.003 but is smaller than or equal to 0.030, the a is greater than 4.0 but is smaller than 5.2, the b is greater than 0.10 but is smaller than 0.3, the c is greater than or equal to 0.04 but is smaller than 0.1, and the d is greater than or equal to 5.6 but is smaller than 7.2 in the formula. The invention further discloses a preparation process of the fluorescent powder. The process uses one of halides of Li, Na, K, Mg, Ca, Sr, Ba, Al, Ga and Ce or a mixture of the two or more halides as a fluxing agent and adopts a staged heating temperature rise mode. At a stage 1, the room temperature T1 is 1400-1600 DEG C, the temperature rise rate is greater than 5 DEG C / min but is smaller than or equal to 10 DEG C / min; at a stage 2, the room temperature T2 is 1850-2000 DEG C, the temperature rise rate is greater than 0 DEG C / min but is smaller than or equal to 5 DEG C / min; after the T2 is reached, heat preservation is performed at the temperature T2 for 8-12 hours. The fluorescent powder emits stronger green light in the emission peak wave length range of 530-540 nm, the half peak width can be controlled to be 50-55 nm, the particle size of the powder is uniform, the luminous performance is good, and the color purity is high. In addition, the method of the beta-SiAlON: Eu2 + green fluorescent powder is simple in process and has low requirements for equipment.

Description

Technical field [0001] The present invention relates to fluorescent powder, specifically a kind of β-SiAlON: Eu 2+ Green phosphor and its synthesis method. Background technique [0002] Since the 1990s, the rapid development of LED technology has made the application of white LED, LED backlight and other fields more and more in-depth and extensive. [0003] Compared with traditional lighting technology, white LED has the advantages of low energy consumption, high efficiency, no pollution, and long life. It has an optimistic future in civil lighting. In LED lighting technology, phosphor is one of its key technologies and raw materials. At present, the commonly used green phosphors for white LEDs are mainly sulfide-based phosphors (such as ZnS: Cu, Al, SrGa 2 S 4 :Eu 2+ ), this kind of phosphors are generally limited in their application due to their low luminous efficiency, poor chemical stability, easy deliquescent, and sulfide gas harmful to the human body and the environment. [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64
CPCC09K11/0883C09K11/7734
Inventor 杨志平董秀芹王海龙赵金鑫
Owner HEBEI LIFU CHEM TECH
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