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Preparation method of fluorescent powder with small particle size

A fluorescent powder, small particle size technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problem of inability to effectively control the particle size and size uniformity of fired products, unable to meet the needs of small-sized LED phosphor powder, and reduce nitrogen Solve the luminous intensity of compound phosphors, achieve high quantum efficiency and luminous efficiency, the preparation method is simple and practical, and the excitation effect is good.

Pending Publication Date: 2021-06-18
西安鸿宇光电技术有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Traditional nitride phosphors are synthesized by high-temperature solid-phase method, which cannot effectively control the particle size and size uniformity of fired products, and cannot meet the needs of small-sized LED phosphors
If a one-time high-intensity ball milling process is used, although nitride phosphors with a particle size D50 (median diameter) of about 10 μm or less can also be obtained, due to the high hardness of nitride phosphor particles, after long-term ball milling, the surface shape will be reduced. Although the particle size of the nitride phosphor is reduced by ball milling, it also has a negative effect, that is, the luminous intensity of the nitride phosphor is significantly reduced.

Method used

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  • Preparation method of fluorescent powder with small particle size
  • Preparation method of fluorescent powder with small particle size
  • Preparation method of fluorescent powder with small particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1 (Ca 0.13 Sr 0.85 )(Al 0.5 Si 0.5 ) 2 N 3 :Eu 0.02

[0057] The raw material that embodiment 1 material adopts is Sr 3 N 2 , Ca 3 N 2 , Si 3 N 4 , AlN, Eu 2 o 3 . And using 0.5wt% porous aluminum fluoride (AlF 3 ) as a flux. Weigh 100 g of the raw materials shown below and mix them.

[0058]

[0059] After weighing the above raw materials, put the powder in a mortar and mix evenly in a glove box (oxygen content<1ppm, water content<1ppm). The mortar is onyx or alumina ceramic. Put the mixed powder into the crucible, compact it lightly, then take it out from the glove box and place it in a high-temperature graphite furnace. The material of the crucible is molybdenum or boron nitride. After the graphite furnace is evacuated and filled with nitrogen, it starts to heat up at a rate of 10°C / min, and the pressure of nitrogen is 1 atmosphere. Heat up to 1800°C and keep warm for 2 hours. After the keep warm, turn off the power and cool down with ...

Embodiment 2

[0082] Example 2 (Ca 0.13 Sr 0.85 )(Al 0.5 Si 0.5 ) 2 N 3 :Eu 0.02

[0083] The raw material that embodiment 1 material adopts is Sr 3 N 2 , Ca 3 N 2 , Si 3 N 4 , AlN, Eu 2 o 3 . And using 0.5wt% porous aluminum fluoride (AlF 3 ) as a flux. Weigh 100 g of the raw materials shown below and mix them.

[0084]

[0085] After weighing the above raw materials, put the powder in a mortar and mix evenly in a glove box (oxygen content<1ppm, water content<1ppm).

[0086] The mortar is onyx or alumina ceramic. Put the mixed powder into the crucible, compact it lightly, then take it out from the glove box and place it in a high-temperature graphite furnace. The material of the crucible is molybdenum or boron nitride. After the graphite furnace is evacuated and filled with nitrogen, it starts to heat up at a rate of 10°C / min, and the pressure of nitrogen is 1 atmosphere. Heat up to 1800°C and keep warm for 2 hours. After the keep warm, turn off the power and cool d...

Embodiment 3

[0088] Example 3 Ca 0.95 (Al 0.5 Si 0.5 ) 2 N3 :Eu 0.005

[0089]

[0090] After weighing the above raw materials, put the powder in a mortar and mix evenly in a glove box (oxygen content<1ppm, water content<1ppm).

[0091] The mortar is onyx or alumina ceramic. Put the mixed powder into the crucible, compact it lightly, then take it out from the glove box and place it in a high-temperature graphite furnace. The material of the crucible is molybdenum or boron nitride. After the graphite furnace is evacuated and filled with nitrogen, it starts to heat up at a rate of 10°C / min, and the pressure of nitrogen is 1 atmosphere. Heat up to 1850°C and keep it warm for 2 hours. After the keep warm, turn off the power and cool down with the furnace. The burnt samples are taken out, crushed, ground, classified, and tested, and put into the jet mill; in the jet mill, the once-fired products are pulverized by an inert gas flow with a pressure of 0.5MPa, and the pulverized samples...

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Abstract

The invention relates to a preparation method of small-particle-size fluorescent powder, and belongs to the field of LED inorganic luminescent materials. The chemical formula of the fluorescent powder material is (Ca, Q) 1-y (Al, Si) 2 (N, T) 3: Ay, and after primary high-temperature roasting, physical crushing and high-temperature heat treatment processes are used, so that the fluorescent powder still has relatively high quantum efficiency and luminous efficiency on the basis of reducing the particle size. The median diameter (particle size D50 data) of the prepared small-particle-size fluorescent powder is 3-7 [mu] m, and the maximum particle size (Dmax) is less than or equal to 15 [mu] m. According to the preparation method, the fluorescent powder with the particle size not larger than 15 microns and the median diameter being 3-7 microns can be obtained, compared with conventional fluorescent powder with the median diameter being 10-30 microns, the quantum efficiency of the fluorescent powder can reach 90% or above, and the fluorescent powder can be applied to the fields of LED illumination, Mini LED and Micro LED backlight display and the like.

Description

technical field [0001] The invention relates to a method for preparing phosphor powder with a small particle size, which belongs to the field of LED inorganic luminescent materials. Background technique [0002] White LED based on GaInN LED (Light Emitting Diode, Light Emitting Diode) is known as the solid-state lighting device in the 21st century. It has the advantages of energy saving, no mercury and other pollution sources, high efficiency, low maintenance cost, long life and small size, etc. Indoor lighting, signal lights, indicator lights, vehicle lights, display screens, advertising screens, outdoor large screens and other fields have gradually replaced traditional light bulbs and fluorescent lamps. [0003] The manufacturing technology of white LED mainly includes: (1) the combination of three kinds of single-color LEDs such as blue, green, and red; (2) blue LED + yellow phosphor; (3) ultraviolet LED + blue, green and red three-color phosphor. In order to obtain high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
CPCC09K11/7728C09K11/7734C09K11/7733C09K11/0883
Inventor 刘德尧张琳王超任守权
Owner 西安鸿宇光电技术有限公司