Low-temperature plasma preparation method of nitride fluorescent powder

A technology of nitride phosphor powder and low-temperature plasma, which is applied in chemical instruments and methods, chemical industry, luminescent materials, etc.

Active Publication Date: 2015-02-04
深圳惠农智光科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, while removing carbon, the high temperature of 500-600°C also has an adverse effect on the phosphor material, such as the oxidation of the matrix and the oxidation of the doped rare earth ions.

Method used

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  • Low-temperature plasma preparation method of nitride fluorescent powder
  • Low-temperature plasma preparation method of nitride fluorescent powder
  • Low-temperature plasma preparation method of nitride fluorescent powder

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Embodiment 1

[0018] A low-temperature plasma preparation method of nitride phosphor powder, the chemical formula of the nitride phosphor powder is Ca 0.98 AlSiN 3 :0.02Eu 2+ , using carbothermal reduction to synthesize nitride phosphor materials under normal pressure, and then using low-temperature plasma carbon removal technology to remove residual carbon in the material, the steps are as follows:

[0019] 1) CaH 2 , AlN, Si 3 N 4 、Eu 2 o 3 According to the general chemical formula, the nano-graphite powder with a purity of 99.5% and an average particle size of 40nm is 0.98:1:0.33:0.01:1.3 in molar ratio, accurately weighed, mixed evenly, and then placed in a boron nitride crucible. Raise the temperature to 1550°C at a rate of 5°C / min in a tube furnace with a nitrogen-hydrogen mixture reducing atmosphere at a ratio of 92:8 at normal pressure and keep it warm for 6 hours. After naturally cooling to room temperature, Ca 0.98 AlSiN 3 :0.02Eu 2+ Nitride phosphor coarse material;

[...

Embodiment 2

[0023] A low-temperature plasma preparation method of nitride phosphor powder, the chemical formula of the nitride phosphor powder is Ca 0.96 AlSiN 3 :0.04Eu 2+ , using carbothermal reduction to synthesize nitride phosphor materials under normal pressure, and then using low-temperature plasma carbon removal technology to remove residual carbon in the material, the steps are as follows:

[0024] 1) CaH 2 , AlN, Si3N4, Eu 2 o 3 According to the general chemical formula, the molar ratio of graphite nano powder with a purity of 99.5% and an average particle size of 40nm is 0.96:1:0.33:0.02:1.4, accurately weighed, mixed evenly, and then placed in a boron nitride crucible. Raise the temperature to 1550°C at a rate of 10°C / min in a tube furnace with a nitrogen-hydrogen mixture reducing atmosphere at a ratio of 92:8 at normal pressure and keep it for 6 hours. After cooling naturally to room temperature, Ca 0.96 AlSiN 3 :0.04Eu 2+ Nitride phosphor coarse material;

[0025] 2) ...

Embodiment 3

[0028] A low-temperature plasma preparation method of nitride phosphor powder, the chemical formula of the nitride phosphor powder is Ca 0.96 AlSiN 3 :0.04Eu 2+ , using carbothermal reduction to synthesize nitride phosphor materials under normal pressure, and then using low-temperature plasma carbon removal technology to remove residual carbon in the material, the steps are as follows:

[0029] 1) Ca0, AlN, Si3N4, Eu 2 o 3According to the general chemical formula, the nano-graphite powder with a purity of 99.5% and an average particle size of 40nm is 0.96:1:0.33:0.02:2.2 in molar ratio, accurately weighed, mixed evenly, and then placed in a boron nitride crucible. Raise the temperature to 1550°C at a rate of 8°C / min in a tube furnace with a nitrogen-hydrogen mixture reducing atmosphere at a ratio of 92:8 at normal pressure and keep it warm for 6 hours, and naturally cool to room temperature to obtain Ca 0.96 AlSiN 3 :0.04Eu 2+ Nitride phosphor coarse material;

[0030] ...

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Abstract

The invention relates to a low-temperature plasma preparation method of nitride fluorescent powder. The chemical general formula of the nitride fluorescent powder is M(1-x)AlSiN3:xEu<2+>, wherein M is Ca, Sr or Ba and x is greater than or equal to 0.005 and less than or equal to 0.20. A nitride fluorescent powder material is synthesized at an ordinary pressure by carbon thermal reduction and residual carbon in the material is removed by adopting a low-temperature plasma decarbonizing technique. The method provided by the invention has the advantages and positive effects that the low-temperature plasma preparation method of the nitride fluorescent powder is relatively simple in preparation condition, raw materials are easily available, the decarbonizing process is efficient and energy-saving, and the nitride fluorescent powder material is prevented from being damaged, so that the production cost of the nitride fluorescent powder is extremely lowered and the light emitting performance of the material is ensured, thereby facilitating popularization and application of the nitride fluorescent powder in the field of illumination and display.

Description

【Technical field】 [0001] The invention relates to the field of phosphor material preparation, in particular to a low-temperature plasma preparation method of nitride phosphor. 【Background technique】 [0002] Nitride phosphors have been widely concerned and applied in the field of lighting and display in recent years due to their excellent luminescent performance, thermal stability and chemical stability which are obviously superior to other phosphor systems. The preparation method of nitride phosphor generally adopts high-temperature pressure firing method, and the firing temperature needs to be above 1600°C, and a nitrogen pressure of 0.1-10MPa is required to prevent Si 3 N 4 Decomposition or oxidation of raw materials. In addition, this high temperature and pressure firing method is also very demanding on raw materials, such as alkaline earth metal nitrides, which are very sensitive to oxygen and moisture in the air, and are easily decomposed and oxidized, so they need t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
CPCY02P20/10
Inventor 王达健李广浩毛智勇孙涛宋维伟卢志娟
Owner 深圳惠农智光科技有限公司
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