Europium doped lanthanide silicon oxynitride and preparation method thereof

A technology of silicon oxynitride and compound, applied in the field of europium-doped lanthanide silicon oxynitride compound and its preparation

Inactive Publication Date: 2013-06-12
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disclosed as CN101434839A is a kind of nitrogen oxide fluorescent powder doped with europium, the chemical general formula of this fluorescent powder is {M (1-x) Eu x } a Si b o c N d , where M is Ba, Sr or Ca, 02 ON:Eu 2+ Phosphor powder and its preparation method are: uniformly mixing raw materials, drying, filtering, calcining and pulverizing to obtain (Ca, Mg)Si which can emit yellow-green light 2 ON:Eu 2+ Phosphor powder; and in the existing research, Eu has not been found 2+ Doping in La-Si-O-N matrix to prepare related reports of fluorescent compounds that can emit blue-green light

Method used

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  • Europium doped lanthanide silicon oxynitride and preparation method thereof
  • Europium doped lanthanide silicon oxynitride and preparation method thereof
  • Europium doped lanthanide silicon oxynitride and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0033] According to chemical formula (La 0.95 Eu 0.05 ) 5 Si 3 o 12 Weighing the molar ratio of each element in N Raw materials: La 2 o 3 Powder 5.004g, SiO 2 Powder 0.8740g, Si 3 N 4 Powder 0.2265g, Eu 2 o 3The powder is 0.2846 g; after mixing, put it in a ball mill, and mill it for 1 hour, take out the ball mill powder, and press it with a tablet machine, the pressure of the tablet machine is 15MPa, the thickness of the tablet is about 11mm, and the diameter is 13mm; the sample is placed in a high-temperature and high-pressure graphite furnace In the middle, fully vacuumize, feed the nitrogen-hydrogen mixed gas source according to the volume ratio of nitrogen and hydrogen at 95:5, raise the temperature to 1250°C, keep warm and sinter for 3 hours; cut off the hydrogen gas source, close the valves of other gas sources, and fill the high Pure nitrogen until the pressure in the furnace is 0.5MPa, heat up to 1550°C, heat-preserve and sinter for 3 hours; open the valve o...

Embodiment 2

[0035] According to chemical formula (La 0.99 Eu 0.01 ) 5 Si 3 o 12 Weighing the molar ratio of each element in N Raw materials: La 2 o 3 Powder 5.002g, SiO 2 Powder 0.8385g, Si 3 N 4 Powder 0.2177g, Eu 2 o 3 Powder 0.0544g; after mixing, put it in a ball mill, ball mill for 1 hour, take out the ball mill powder, and press it with a tablet machine. In the middle, fully vacuumize, feed the nitrogen-hydrogen mixed gas source according to the volume ratio of nitrogen and hydrogen at 95:5, raise the temperature to 1250°C, keep warm and sinter for 3 hours; cut off the hydrogen gas source, close the valves of other gas sources, and fill the high Pure nitrogen until the pressure in the furnace is 0.5MPa, heat up to 1450°C, heat-preserve and sinter for 3 hours; open the valve of the outlet pipe, reduce the pressure in the furnace to normal pressure, open the valve of the inlet pipe, and make the volume ratio of nitrogen and hydrogen 95:5 Introduce nitrogen and hydrogen mixe...

Embodiment 3

[0037] According to chemical formula (La 0.9 Eu 0.1 ) 5 Si 3 o 12 Weighing the molar ratio of each element in N Raw materials: La 2 o 3 Powder 5.0002 g, SiO 2 Powder 0.9022g, Si 3 N 4 Powder 0.2390g, Eu 2 o 3 0.6000 g of powder; after mixing, put it in a ball mill and mill it for 1 hour, take out the ball mill powder, and press it with a tablet machine. In the middle, fully vacuumize, feed the nitrogen-hydrogen mixed gas source according to the volume ratio of nitrogen and hydrogen at 95:5, raise the temperature to 1250°C, keep warm and sinter for 3 hours; cut off the hydrogen gas source, close the valves of other gas sources, and fill the high Pure nitrogen until the pressure in the furnace is 0.5MPa, heat up to 1500°C, heat-preserve and sinter for 3 hours; open the valve of the outlet pipe, reduce the pressure in the furnace to normal pressure, open the valve of the inlet pipe, and set the volume ratio of nitrogen and hydrogen to 95:5 Introduce nitrogen and hydrog...

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Abstract

The invention discloses a europium doped lanthanide silicon oxynitride, of which the chemical general formula is La5-5xEu5xSi3O12N, wherein x is more than 0 and less than 0.25. The preparation method comprises the steps of: (a) weighing raw materials: lanthanum trioxide, silicon dioxide, silicon nitride and europium oxide, according to the molar ratio of the chemical formula La5-5xEu5xSi3O12N (x is more than 0 and less than 0.25); (b) ball-milling the raw materials and tabletting; (c) putting tablets into a high temperature furnace, under the nitrogen hydrogen atmosphere, raising the furnace temperature to 1000-1250 DEG C, and sintering for 3-10 hours; (d) turning off a hydrogen source, under the environment of charging nitrogen gas, keeping the high temperature furnace at a pressure of 0.5-1MPa, raising the furnace temperature to 1450-1550 DEG C, and continuously sintering the tablets for 3-10 hours; and (e) ventilating to release the pressure in the furnace to be an ordinary pressure, cooling down the high temperature furnace to room temperature by circulating under the nitrogen-hydrogen mixed atmosphere, taking out the sample tablets, and grinding, thus obtaining a fluorescent material. The fluorescent material prepared by the preparation method is stable in physicochemical property, convenient to control luminescence property, simple in preparation method, and free from environmental pollution, and is applicable to industrialized mass production.

Description

technical field [0001] The invention relates to a fluorescent material containing rare earth metals and a preparation method thereof, in particular to a europium-doped lanthanide silicon oxynitride compound and a preparation method thereof. Background technique [0002] White light LED has attracted widespread attention due to its small size, energy saving, environmental protection, long life and other advantages, and is called a new generation of lighting sources. At present, white light LED lighting is mainly realized through light conversion, that is, through blue light chips to excite yellow phosphor powder, blue and yellow light are mixed to obtain white light, or purple light (or ultraviolet light) is used to excite red, green, and blue phosphor powder, red, green, and blue phosphors. Green and blue light mix into white light. For this reason, technicians have developed a variety of fluorescent materials capable of displaying various colors of visible light under ligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/79
Inventor 鲁法春白利静杨志平李志强刘玉峰
Owner HEBEI UNIVERSITY
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