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Nitride red luminous material with long afterglow and preparation method thereof

A technology of long-lasting luminescence and nitrides, which is applied in the direction of luminescent materials, chemical instruments and methods, etc. It can solve the problems of easy volatilization of elemental sulfur, monotonous luminous color, poor chemical stability, etc., and achieve easy acquisition, high luminous intensity, and stability good sex effect

Inactive Publication Date: 2014-03-26
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of aluminate long afterglow materials is that the luminous color is monotonous, the emission spectrum is mainly concentrated in the range of 440-520nm, and it is unstable when exposed to water. Coating treatment is often used to improve its water resistance
[0004] Alkaline-earth aluminate green and blue long-lasting phosphors doped with rare earth ions have entered the application stage, while red long-lasting phosphors have not been able to meet the needs of applications, mainly because indicators such as luminous brightness and afterglow time are different from those of yellow-green and There is a big gap in the blue long afterglow phosphor
Chinese patents 200910026093.4 and 201210597523.X report red long-lasting luminescent material Y 2 o 2 S:Eu 3+ , Ti 4+ ,Mg 2+ , its emission wavelength is around 625nm, and the afterglow time can reach 3.5 hours, but it is easy to volatilize elemental sulfur during the synthesis process, and at the same time, it has poor chemical stability and is easy to deliquescence
Chinese patent 201210227650.0 reports a nitride red long-lasting phosphor, which has good chemical stability, high luminous efficiency, and long afterglow time, but it uses nitride raw materials and glove boxes to mix, and there are disadvantages such as high raw material cost and complicated process.

Method used

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  • Nitride red luminous material with long afterglow and preparation method thereof
  • Nitride red luminous material with long afterglow and preparation method thereof

Examples

Experimental program
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Effect test

example 1

[0021] According to chemical formula Sr 1.99 Si 5 N 8 : 0.005Eu, 0.005Tm stoichiometric ratio, accurate weighing of SrCO 3 (99.9%), Si 3 N 4 (99.9%), Eu 2 o 3 (99.99%), Tm 2 o 3 (99.99%) raw material, the molar ratio of the addition amount of anhydrous glucose and strontium carbonate is 1:6.

[0022] Put the above-mentioned weighed raw materials in an agate mortar, add an appropriate amount of alcohol as a grinding medium, grind for 30-60 minutes to mix the raw materials evenly, then put them in a drying oven for 4 hours at 80°C, then put them into a graphite crucible, Heating in a tube furnace, raising the temperature to 600-700°C at a rate of 8°C / min, keeping it for 2.5 hours, then raising it to 1500-1600°C at a rate of 5°C / min, keeping it at a temperature of 5-6 hours, and then heating it at a temperature of 5-6 hours Cool down to 250°C at a cooling rate of 10°C / min, and cool down to room temperature with the furnace. After the calcined product is ground, it is pi...

example 2

[0024] According to chemical formula Sr 1.97 Si 5 N 8 : 0.01Eu, 0.02Tm stoichiometric ratio, accurate weighing of SrCO 3 (99.9%), Si 3 N 4 (99.9%), Eu 2 o 3 (99.99%), Tm 2 o 3 (99.99%) raw material, the molar ratio of the addition amount of anhydrous glucose and strontium carbonate is 1:6.

[0025] The mixing process and steps are consistent with Example 1. Put the sample into a tube furnace, raise the temperature to 600-700°C at a rate of 8°C / min, keep it for 2.5 hours, then raise it to 1500-1600°C at a rate of 5°C / min, keep it for 5-6 hours, and then Cool down to 250°C at a cooling rate of 5-10°C / min, and cool down to room temperature with the furnace. After the calcined product is ground, it is pickled with hydrochloric acid with a concentration of 1-20wt%, washed with deionized water, and repeated 5-8 times, and dried to obtain a nitride red long-lasting luminescent material.

example 3

[0027] According to chemical formula Sr 1.93 Si 5 N 8 : 0.02Eu, 0.05Tm stoichiometric ratio, accurate weighing of SrCO 3 (99.9%), Si 3 N 4 (99.9%), Eu 2 o3 (99.99%), Tm 2 o 3 (99.99%) raw material, the molar ratio of the addition amount of anhydrous glucose and strontium carbonate is 1:6.

[0028] The mixing process and steps are consistent with Example 1. Put the sample into a tube furnace, raise the temperature to 600-700°C at a rate of 8°C / min, keep it for 2.5 hours, then raise it to 1500-1600°C at a rate of 5°C / min, keep it for 5-6 hours, and then Cool down to 250°C at a cooling rate of 5-10°C / min, and cool down to room temperature with the furnace. After the calcined product is ground, it is pickled with hydrochloric acid with a concentration of 1-20wt%, washed with deionized water, and repeated 5-8 times, and dried to obtain a nitride red long-lasting luminescent material.

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Abstract

The invention discloses a nitride red luminous material with long afterglow and a preparation method thereof. The material has a chemical formula of M<2-x-y>Si5N8:xEu,yRe, wherein in the formula, M is one or more elements selected from Sr, Ca, and Ba, x is more than or equal to 0.005 and less than or equal to 0.15, y is more than or equal to 0.005 and less than or equal to 0.15, and Re represents at least one element selected from the following elements: Tm, Dy, Pr, Nd, Sm, Gd, and Lu. The material comprises at least two rare earth elements. The preparation method obtains a red luminous material with long afterglow, which has the advantages of good chroma, high brightness, and long afterglow time, has the advantages of simple technology, available raw materials, and low cost, and obtains a nitride red luminous material with long afterglow.

Description

technical field [0001] The invention relates to the technical field of rare earth luminescent materials, in particular to a nitride red long-lasting luminescent material and a preparation method. Background technique [0002] Rare earth long afterglow luminescent material is a new type of energy-saving and environmentally friendly material. It can absorb the energy of sunlight or light, store part of the energy, and then slowly release it in the form of visible light. This feature can be widely used in lighting, indication and decoration, etc. In recent years, it has been gradually extended to high-tech fields such as information storage, radiation detection and imaging display. [0003] Traditional long afterglow materials are mainly zinc sulfide (ZnS:Cu) and alkaline earth sulfides (CaS:Bi, Ca, SrS:Bi). Although rare-earth-activated sulfide long-lasting luminescent materials have the advantages of bright body color, fast absorption under weak light, and various luminous c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/59
Inventor 黄得财周有福许文涛向明
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI