Europium ion activated silicon phosphate green fluorescent powder and its preparation method

A green phosphor, silicophosphate technology, applied in the field of ultraviolet-near ultraviolet type white light LED, can solve the problems of poor stability that cannot meet the requirements of white light LED applications, poor luminescence stability of phosphors, easy deliquescence, etc., and is suitable for continuous Chemical production, good luminous intensity, not easy to deliquescence effect

Inactive Publication Date: 2014-07-30
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the green fluorescent powder of the sulfide system has high conversion characteristics, but its disadvantages are very obvious. This kind of fluorescent powder has poor luminous stability, large light attenuation, high cost, and is easy to deliquescence, among which the stability is poor. Can not meet the requirements of white LED applications

Method used

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  • Europium ion activated silicon phosphate green fluorescent powder and its preparation method
  • Europium ion activated silicon phosphate green fluorescent powder and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Implementation Example 1: Ca 4.9875 (PO 4 ) 2 SiO 4 : 0.0125Eu 2+ preparation of

[0026] First, according to the chemical formula Ca 4.9875 (PO 4 ) 2 SiO 4 : 0.0125Eu 2+ The stoichiometric ratio of the reaction raw material Eu 2 o 3 , CaO, SiO 2 , NH 4 h 2 (PO 4 ) in a molar ratio of 0.00625: 4.9875: 1: 2, after ball milling for 24 hours and mixing uniformly, the mixture was put into a crucible for the first calcination, the calcination temperature was 600°C, and the calcination time was 6 hours; naturally cooled to room temperature After that, remove the sample. After the raw materials calcined for the first time are ball-milled and mixed evenly again, the mixture is put into a crucible and calcined for the second time under a nitrogen-hydrogen mixed reducing atmosphere. The calcining temperature is 1300°C, and the calcining time is 8 hours. The sample was post-processed to obtain silicon phosphate green phosphor.

Embodiment 2

[0027] Implementation Example 2: Ca 4.975 (PO 4 ) 2 SiO 4 : 0.025Eu 2+ preparation of

[0028] First, according to the chemical formula Ca 4.975 (PO 4 ) 2 SiO 4 : 0.025Eu 2+ The stoichiometric ratio of the reaction raw material Eu(NO 3 ) 3 , CaCO 3 , SiO 2 , (NH 4 ) 3 (PO 4 ) in a molar ratio of 0.025: 4.975: 1: 2, after ball milling for 24 hours and mixing uniformly, the mixture was put into a crucible for the first calcination, the calcination temperature was 650°C, and the calcination time was 5 hours; naturally cooled to room temperature After that, remove the sample. After the raw materials calcined for the first time are ball milled and mixed evenly again, the mixture is put into a crucible and calcined for the second time under a mixed reducing atmosphere of nitrogen and hydrogen. The calcining temperature is 1350°C, and the calcining time is 7 hours. The sample was post-processed to obtain silicon phosphate green phosphor.

Embodiment 3

[0029] Implementation Example 3: Ca 4.95 (PO 4 )2 SiO 4 : 0.05Eu 2+ preparation of

[0030] First, according to the chemical formula Ca 4.95 (PO 4 ) 2 SiO 4 : 0.05Eu 2+ The stoichiometric ratio of the reaction raw material Eu 2 o 3 , CaCO 3 , SiO 2 , NH 4 h 2 (PO 4 ) in a molar ratio of 0.025: 4.95: 1: 2, after ball milling for 24 hours and mixing uniformly, the mixture was put into a crucible for the first calcination, the calcination temperature was 700°C, and the calcination time was 4 hours; naturally cooled to room temperature After that, remove the sample. After the raw materials calcined for the first time are ball-milled and mixed evenly again, the mixture is put into a crucible and calcined for the second time under a nitrogen-hydrogen mixed reducing atmosphere. The calcining temperature is 1400°C, and the calcining time is 7 hours. The sample was post-processed to obtain silicon phosphate green phosphor.

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Abstract

The invention belongs to the technical field of rare earth luminescent materials, and relates to a europium ion activated silicon phosphate green fluorescent powder and its preparation method. The green fluorescent powder has the following chemical components shown in the following chemical formula: M5-x (PO4) 2SiO4:xEu <2 +>, where M element is one or more from Ca, Mg, Sr or Ba, 0.001 <=x <= 0.1, M5-x (PO4) 2SiO4 is a matrix, Eu <2 +>is a doped rare earth ion. The silicon phosphate green fluorescent powder M5-x (PO4) 2SiO4:xEu <2 +> is synthesized by a high temperature solid phase synthesis method, under excitation of near UV (ultra violet), the silicon phosphate green fluorescent powder has a strong absorption in the range of excitation wavelength of 220-450nm, has a wider emission peak in the range of 430-700nm, is suitable for excitation of near UV of 350-430nm, and is very consistent in emission wavelength with a near ultraviolet semiconductor chip; the silicon phosphate green fluorescent powder has the advantages of high luminous efficiency, high strength and stable chemical property, and is in a green light wave band; the preparation method of europium ion activated silicon phosphate is simple and easy to operate and can be used in industrial production, and the europium ion activated silicon phosphate green fluorescent powder can be used in high color rendering white-light LED, and ahs excellent application prospects in solid state lighting field.

Description

technical field [0001] The invention relates to a europium ion-activated silicon phosphate green fluorescent powder and a preparation method thereof, in particular to a fluorescent powder emitting green fluorescence under near-ultraviolet light excitation, which can be applied to ultraviolet-near ultraviolet white light LEDs and belongs to Fluorescent material technical field. Background technique [0002] White light-emitting diode (LED) is called the fourth generation of lighting source. As a new generation of solid light source, in addition to overcoming the shortcomings of traditional incandescent and fluorescent lamps such as high energy consumption, fragility, and pollution, it also has small size and environmental protection. , fast response, long life, planar packaging, high luminous intensity, high efficiency, energy saving, vibration resistance, low voltage drive, and no environmental pollution. Therefore, white LEDs are widely used in various lighting facilities ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/71
CPCY02B20/00
Inventor 魏健沈常宇刘桦楠路艳芳陈德宝
Owner CHINA JILIANG UNIV
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