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A kind of nitride fluorescent powder and preparation method thereof

A nitride phosphor, aluminum nitride technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of high cost of phosphor, poor chemical stability, chip damage, etc., to improve luminescence performance, chemical performance stability, The effect of high luminous efficiency

Active Publication Date: 2018-01-09
JIANGMEN KANHOO IND
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Problems solved by technology

[0003] There are many kinds of red phosphors for LEDs that have been reported, the earliest being Eu 2 + Activated SrS, CaS series, but poor chemical stability at high temperature, easy to decompose to produce sulfur, which is very harmful to the chip; Eu 3+ activated-CaMoO 4 , Y(V,P)O 4 series, its excitation efficiency is relatively low in the near-ultraviolet and blue light regions, and the excitation spectra are some sharp line spectra in the near-ultraviolet and visible light regions, which increases the difficulty of screening matching chips; in addition, Mn 4+ Activated 3.5MgO 0.5MgF 2 · GeO 2 and 6MgO·As 2 o 5 However, these two phosphors are expensive and toxic, which restricts their application in white LEDs; in order to improve the performance of phosphors and meet the needs of white LEDs, it is necessary to find red phosphors suitable for LED chips, and nitride Phosphor powder has high luminous efficiency, wide half-peak width, stable chemical properties, safety and non-toxicity, and has attracted widespread attention

Method used

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  • A kind of nitride fluorescent powder and preparation method thereof
  • A kind of nitride fluorescent powder and preparation method thereof
  • A kind of nitride fluorescent powder and preparation method thereof

Examples

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preparation example Construction

[0039] According to a second aspect of the present invention, a method for preparing a nitride phosphor is provided, comprising the following steps:

[0040] 1) According to chemical formula M p Q q N 3 The stoichiometric ratio of xR takes by weighing the nitride or oxide of M, the nitride or oxide of Q, the oxide of R, wherein: M is at least one in B, Al, Ga, Y, La; Q is At least one of Si, Ge, Ti, Sn; R is at least one of Eu, Ce, Li, Na, K; 0.8≤p≤1.5; 0.9≤q≤1.2; 0.001≤x≤0.2; Flux, the weighed raw materials are poured into the jet mill for jet milling to obtain the mixture M p Q q N 3 :xR;

[0041] 2) Press chemical formula A under protective atmosphere 1-x m p Q q N 3 : The stoichiometric ratio of xR Continue to weigh the mixture M p Qq N 3 : Nitride of xR and A, A is at least one of Be, Mg, Ca, Sr, Ba; add 0.001 to 0.03% by weight of silicon powder to prepare a mixture, and place the mixture in a vacuum ball milling tank, Add ball milling beads and mill evenly;...

Embodiment 1

[0047] Example 1 Mg 0.005 Sr 0.090 Ca 0.865 AlSiN 3 :0.040Eu

[0048] 1) According to the chemical formula AlSiN 3 : The stoichiometric ratio of 0.040Eu weighs 4098.8g aluminum nitride, 4676.1g α-silicon nitride, 703.9g europium oxide, adds 148.3g strontium fluoride and 148.3g calcium fluoride as flux, and pours the weighed raw materials into The jet mill was used for jet milling, the air flow rate of the jet mill was 0.8 MPa, and the mixture A1 was obtained after jet milling for 5 hours.

[0049] 2) Under the protective atmosphere of high-purity nitrogen in a vacuum glove box, weigh 0.168g of magnesium nitride, 8.726g of strontium nitride, 42.745g of calcium nitride, and 0.298g of silicon powder, and place them in a vacuum ball milling tank with 97.754g of mixture A1. 149 g of zirconia beads were added, the rotation speed was 300 rpm, and the mixture B1 was obtained after ball milling for 4 hours.

[0050] 3) Put the mixture B1 under a nitrogen protective atmosphere, ap...

Embodiment 2

[0053] Example 2 Sr 0.255 Ca 0.700 al 0.992 Ga 0.008 SiN 3 :0.045Eu

[0054] 1) According to the chemical formula AlSiN 3 : The stoichiometric ratio of 0.045Eu takes by weighing 4066.0g aluminum nitride, 75.0g gallium oxide, 4676.1g α-silicon nitride, 791.8g europium oxide, adds 157.2g strontium fluoride and 157.2g calcium fluoride as flux, will weigh The raw materials taken were poured into a jet mill for jet milling, the air flow rate of the jet milling was 1 MPa, and the mixture A2 was obtained after jet milling for 6 hours.

[0055] 2) Under the protective atmosphere of high-purity nitrogen in a vacuum glove box, weigh 24.724g of strontium nitride, 34.591g of calcium nitride, and 0.477g of silicon powder, and place them in a vacuum ball mill jar with 99.233g of mixture A2, and add 159g of zirconia beads, The rotational speed was 200 rpm, and after ball milling for 3 hours, mixture B2 was obtained.

[0056] 3) Put the mixture B2 under a nitrogen protective atmosphere...

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Abstract

The invention discloses a nitride phosphor and a preparation method thereof. The chemical composition is: A1‑xMpQqN3:xR, and also discloses a preparation method of the nitride. The excitation spectrum of the phosphor of the present invention is broadband excitation, covering Near-ultraviolet and blue light match well with the emission spectrum of the LED chip. The phosphor emits red light, with high luminous efficiency, wide half-peak width, and stable chemical properties. The phosphor spectrum is adjustable. By changing the ratio of metal elements in A1‑xMpQqN3:xR, the emission peak wavelength can be moved from 610nm to 665nm. The phosphor powder can also be added with high-purity ultrafine silicon powder to remove the adsorbed oxygen contained in the silicon nitride, reduce the oxygen content of the phosphor powder of the present invention, and improve the luminescent performance of the phosphor powder.

Description

technical field [0001] The invention relates to the field of rare earth luminescent materials, in particular to a nitride fluorescent powder and a preparation method thereof. Background technique [0002] As a new type of solid-state lighting product, white light LED has attracted much attention. White light LED has the advantages of high luminous efficiency, long life, low energy consumption, fast response speed, and no pollution. It has great development potential in the lighting market. Therefore, white light LED LEDs are regarded as essential solid-state lighting sources. At present, the traditional method widely used in the preparation of white LEDs is blue light produced by InGaN chips and yellow phosphor (YAG:Ce 3+ ) combined to produce white light, the preparation and processing of this method is simple and mature, however, the white light LED manufactured by this traditional method has poor color temperature stability and poor color rendering. However, the above-m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64C09K11/66
Inventor 梁志娟陈伟李云锋冯荣标万国江陈涛张洪峰
Owner JIANGMEN KANHOO IND
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