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A kind of rare earth ion doped zirconium niobate fluorescent powder and its preparation method

A technology of rare earth ions and phosphors, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of harsh production equipment, easy decomposition, low luminous efficiency, etc., to achieve low production conditions and equipment requirements, and no pollution to the environment. , the effect of high luminous intensity

Active Publication Date: 2018-04-20
徐州博创建设发展集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Example: someone tries to convert Y 2 o 2 S:Eu 3+ Applied in the WLED field, however, the current commercial red phosphor Y 2 o 2 S:Eu 3+ There are many disadvantages: low luminous efficiency under near-ultraviolet light excitation, unstable chemical properties, easy to decompose, short life, and the precipitation of sulfur will cause corrosive effects on the chip, resulting in the failure of the entire device
Among them, rare earth-activated nitrogen oxides are highly stable and have good luminous efficiency, such as: Sr 2 Si 5 N 8 :Eu 2+ 、SrSi 2 o 2 N 2 :Eu 2+ , but the matrix synthesis of this type of material needs to be completed at high temperature (1600-1700°C) and high nitrogen or ammonia pressure (10atm), which has very strict requirements on production equipment

Method used

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  • A kind of rare earth ion doped zirconium niobate fluorescent powder and its preparation method
  • A kind of rare earth ion doped zirconium niobate fluorescent powder and its preparation method
  • A kind of rare earth ion doped zirconium niobate fluorescent powder and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] According to the chemical formula Zr 6 Nb 2 o 17 : 0.0001Eu weighed zirconia ZrO 2 : 7.392 g, europium oxide Eu 2 o 3 : 0.001 g, niobium pentoxide Nb 2 o 5 : 2.658 grams, add an appropriate amount of acetone to the agate mortar, mix and grind evenly, then pre-calcine in the air atmosphere, calcined at 350 ° C for 4 hours and cool in the furnace, take out the sample and use the same method again for the pre-calcined raw materials Thoroughly mix and grind evenly, then calcined again in air atmosphere, calcined at 750°C for 4 hours, cooled to room temperature, and took out the sample. Mix and grind evenly again, and finally calcinate at 1150°C for 4 hours in an air atmosphere, cool to room temperature, take it out and grind it thoroughly to obtain a sample.

[0036] see figure 1 , is the X-ray powder diffraction pattern of the sample prepared by the technical scheme of this embodiment; the XRD test results show that the prepared sample has good crystallinity and is...

Embodiment 2

[0042] According to the chemical formula Zr 6 Nb 2 o 17 : 0.01Eu Weigh zirconium nitrate Zr (NO 3 ) 4 ·5H 2 O: 6.433 g, europium carbonate Eu 2 (CO 3 ) 3 : 0.004 g, niobium hydroxide Nb(OH) 5 : 0.890 g, add an appropriate amount of acetone to the agate mortar, mix and grind evenly, then pre-calcine in the air atmosphere, pre-calcine at 300 ° C for 2 hours and cool in the furnace, take out the sample and use the same pre-calcined raw material again Methods Mix well and grind evenly, then calcined again in air atmosphere, calcined at 700°C for 2 hours, cooled to room temperature, and took out the sample. Mix and grind evenly again, and finally calcinate at 1100°C for 2 hours in an air atmosphere, cool to room temperature, take it out and grind it thoroughly to obtain a sample.

[0043] The X-ray powder diffraction pattern, excitation spectrum, fluorescence spectrum, luminescence decay curve, and scanning electron micrograph of the sample prepared by the technical scheme...

Embodiment 3

[0045] According to the chemical formula Zr 6 Nb 2 o 17 : 0.01Eu Weigh zirconium hydroxide Zr(OH) 4 : 3.153 g, europium nitrate Eu (NO 3 ) 3 ·6H 2 O: 0.089 g, niobium chloride NbCl 5 : 1.801 g, add an appropriate amount of acetone to the agate mortar, mix and grind evenly, then pre-calcine in the air atmosphere, pre-calcine at 700 ° C for 12 hours and cool in the furnace, take out the sample and use the same pre-calcined raw material again Methods Mix well and grind evenly, then calcined again in air atmosphere, calcined at 1100°C for 12 hours, cooled to room temperature, and took out the sample. Grind again evenly, and finally calcined at 1500°C for 12 hours in an air atmosphere, cooled to room temperature, and fully ground after taking out to obtain a sample.

[0046] The X-ray powder diffraction pattern, excitation spectrum, fluorescence spectrum, luminescence decay curve, and scanning electron micrograph of the sample prepared by the technical scheme of this embodim...

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Abstract

The invention relates to a rare earth ion-doped zirconium niobate fluorescent powder and a preparation method thereof. A chemical formula of the fluorescent powder is Zr6Nb2O17:xEu, wherein x is the molar percentage of Eu3+ doping, and x is greater than or equal to 0.0001 and is smaller than or equal to 0.5; a high-temperature solid phase method or chemical synthesizing method is adopted, zirconium niobate is used as a substrate, and the rare earth ions are added, so as to prepare the fluorescent powder. The rare earth ion-doped zirconium niobate fluorescent powder has the advantages that the light emitting intensity is high, the stability is good, the ultraviolet light near 267 nanometer can be absorbed, the red light near 613 nanometer is converted and emitted, and the fluorescent powder can be applied to prepare LED (light emitting diode) illumination devices; the preparation method is simple, the operation is easy, the protection by special gas is not needed, the requirement on production conditions and equipment is low, the production cost is low, the exhaust of waste gas and waste liquid is avoided, the environment-friendly effect is realized, and the pollution is avoided.

Description

technical field [0001] The invention relates to a fluorescent material and a preparation method thereof, in particular to a rare earth ion-doped zirconium niobate fluorescent powder and a preparation method thereof, belonging to the field of inorganic light-emitting materials. Background technique [0002] With the aggravation of global environmental problems and energy shortage, energy conservation and environmental protection have become an important issue that people are currently facing. In the field of general lighting, white LED products have become the focus of attention. It is a new type of green and environmental protection lighting product, which has the advantages of high electro-optic efficiency, small size, low power, long life, etc. It is considered as a new generation of lighting source and has a good development trend. [0003] There are two main ways for white LEDs to produce white light: the first is to combine red, green, and blue LEDs to produce white li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/67
CPCC09K11/7728
Inventor 乔学斌
Owner 徐州博创建设发展集团有限公司