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Long-wavelength high-brightness nitride red fluorescent powder and preparation method thereof

A technology of red fluorescent powder and red fluorescence, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low luminous intensity, achieve high luminous efficiency, stable performance, and broad market prospects

Inactive Publication Date: 2015-06-03
辽宁法库陶瓷工程技术研究中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The wavelength of the existing red phosphors is mostly concentrated around 600nm, mainly orange-red, and the luminous intensity is low, so it is necessary to develop long-wavelength and high-intensity red phosphors

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] According to the chemical formula Ca 0.8 Sr 0.15 AlSiN 3 : 0.05Eu 2+ The stoichiometric ratio, accurately weigh the following raw materials CaCO 3 (99.99%), SrCO 3 (99.99%), AlN (99.9%), Si 3 N 4 (99.9%), Eu 2 o 3 (99.99%), adding 3% of the total mass of raw materials BaF 2 As a flux, put the above raw materials into a ball mill tank, add polyethylene glycol 600 with 5% of the total mass of the powder, and ball mill for 1 hour to make the materials evenly mixed, put them into a graphite crucible and put them in a high-temperature tube furnace, pump Inject 95%N after vacuum 2 -5%H 2 of the gas mixture. During low-temperature calcination, the tube furnace was raised to 700°C at a rate of 8°C / min, and held for 3 hours. When roasting at high temperature, N 2 The gas is raised to 1700°C at a rate of 3°C / min, and kept at this temperature for 12 hours, then cooled to room temperature with the furnace. After ball milling and sieving the roasted product, it was pic...

example 2

[0026] According to the chemical formula Ca 0.77 Ba 0.2 AlSiN 3 : 0.03Eu 2+ The stoichiometric ratio, accurately weigh the raw material CaCO 3 (99.99%), BaCO 3 (99.99%), AlN (99.9%), Si 3 N 4 (99.9%), Eu 2 o 3 (99.99%), add NaF of 5% of the total mass of raw materials as a flux, put the above-mentioned raw materials into a ball mill jar, add polyethylene glycol 400 of 7% of the total mass of powder, and ball mill for 1 hour to make the materials mix uniformly, Put it into a graphite crucible and put it into a high-temperature tube furnace for roasting and vacuuming, then feed 80%N 2 -20%H 2 When roasting at a low temperature, the tube furnace was raised to 800°C at a rate of 8°C / min and kept for 2 hours. When roasting at high temperature, N 2 The gas is raised to 1600°C at a heating rate of 3°C / min, kept at this temperature for 8 hours, and then cooled to room temperature with the furnace. After ball milling and sieving the roasted product, it was pickled with 10% ...

example 3

[0028] According to the chemical formula Ca 0.75 Sr 0.1 Ba 0.1 AlSiN 3 : 0.05Eu 2+ The stoichiometric ratio, accurately weigh the raw material CaCO 3 (99.99%), SrCO 3 (99.99%), BaCO 3 (99.99%), AlN (99.9%), Si 3 N 4 (99.9%), Eu 2 o 3 (99.99%), adding 4% of the total mass of raw materials NH 4F is used as a flux, put the above raw materials into a ball mill tank, add polyethylene glycol 600 with 6% of the total mass of the powder, and ball mill for 2 hours to make the materials evenly mixed, put them into a graphite crucible and put them into a high-temperature tube furnace for pumping Inject 90%N after vacuum 2 -10%H 2 When roasting at a low temperature, the tube furnace was raised to 700°C at a rate of 10°C / min and kept for 2.5 hours. When roasting at high temperature, N 2 The gas is raised to 1800°C at a rate of 2°C / min, and kept at this temperature for 10 hours, then cooled to room temperature with the furnace. After ball milling and sieving the calcined prod...

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Abstract

The invention provides long-wavelength high-brightness nitride red fluorescent powder and a preparation method thereof. The chemical composition of the fluorescent powder system is Ca1-x-yMxAlSiN3:yEu<2+>, wherein M is one or two of Ba and Sr, x is more than or equal to 0 and less than or equal to 0.5, and y is more than or equal to 0.001 and less than or equal to 0.5. The nitride red fluorescent powder provided by the invention is prepared by adopting a carbon thermal reduction nitriding process, and polyethylene glycol is used as a reducing agent and is carbonized by virtue of low-temperature calcination, so that the problem that a product contains residues by using graphite powder as the reducing agent can be avoided. By adopting the preparation method, the nitride red fluorescent powder, which is stable in performance, high in luminous efficiency, and adjustable in emission peak in a range of 640-680nm, can be prepared.

Description

technical field [0001] The invention relates to a nitride red phosphor powder for a light emitting diode (LED) and a preparation method thereof, belonging to the technical field of solid light emitting materials. Background technique [0002] As a new type of solid-state light source, white LED has the advantages of energy saving, environmental protection, and high efficiency compared with traditional incandescent and fluorescent lamps, and is known as the fourth-generation green light source. At present, white light LEDs for lighting use blue light chips to excite YAG: Ce 3+ Yellow fluorescent powder is used to achieve this. The LED produced by this method has a high color temperature and a low color rendering index. It is difficult to obtain white light that is pure and comfortable for the human eye. In order to improve the color rendering index of white LEDs, the industry usually adds a small amount of red phosphor powder to yellow powder to obtain pure and comfortable w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
Inventor 刘娇娜韩绍娟许壮志薛健张明杨殿来
Owner 辽宁法库陶瓷工程技术研究中心
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