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Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof

A nitrogen oxide and phosphor technology, applied in the field of rare earth luminescent materials, can solve problems such as the condition of excellent light source, color temperature change, color temperature rise, etc., and achieve the advantages of industrialized large-scale production, improved luminous intensity and performance, and low cost. Effect

Inactive Publication Date: 2013-03-20
CHONGQING ACADEMY OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the white light emitted by white LEDs is all cool white light, and the solubility requirements for dopant ions are also very strict. In order to convert this cold white light into warm white light, the existing technology uses a mixture of two or more types of phosphors. However, due to the different attenuation degrees of different phosphors, the color temperature will continue to change, and usually the color temperature will increase, so that this kind of warm white LED does not have the conditions for an excellent light source

Method used

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  • Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof
  • Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof
  • Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 Preparation of Sr 0.98 Si 2 o 2 N 2 :0.02Eu 2+ Phosphor powder

[0035] Weigh 4.3403g SrCO 3 (AR), 2.8056g Si 3 N 4 (purity>95%) and 0.1056g Eu 2 o 3 (purity>99.99%), after mixing, put it in a zirconia ball mill jar, add zirconia balls and an appropriate amount of ball milling medium, the total amount of the sample should not exceed 2 / 3 of the ball mill jar, and ball mill it on a planetary ball mill for 3 hours; The samples were put into a drying oven and dried at 100°C for 4 hours; the dried powder was placed in an atmosphere furnace and filled with N 2 / H 2 The mixed gas is circulated, the calcination temperature is 1300°C, and the calcination time is 5 hours; with the furnace cooling, the sample is taken out, ground and sieved, and the spectrum is tested as follows: figure 1 shown.

[0036] Such as figure 1 The fluorescent powder shown can be effectively excited by ultraviolet light, near ultraviolet light and blue light in the range of 250-5...

Embodiment 2

[0037] Example 2 Preparation of Sr 0.96 Si 2 o 2 N 2 :0.04Eu 2+ Phosphor powder

[0038] Weigh 4.2517g SrCO 3 (AR), 2.8056g Si 3 N 4 (purity>95%) and 0.2112g Eu 2 o 3 (purity>99.99%), after mixing, put it in a zirconia ball mill jar, add zirconia balls and an appropriate amount of ball milling medium, the total amount of the sample should not exceed 2 / 3 of the ball mill jar, and ball mill it on a drum mill for 3 hours; The samples were put into a drying oven and dried at 100°C for 4 hours; the dried powder was placed in an atmosphere furnace and filled with N 2 / H 2 The mixed gas is circulated, the calcination temperature is 1500°C, and the calcination time is 2 hours; with the furnace cooling, the sample is taken out, ground and sieved, and the spectrum is tested as follows: figure 2 shown.

[0039] Such as figure 2 The fluorescent powder shown can be effectively excited by ultraviolet light, near ultraviolet light and blue light in the range of 250-500nm to ...

Embodiment 3

[0040] Example 3 Preparation of Sr 0.98 Si 2 o 2 N 2 :0.02Eu 2+ Phosphor powder

[0041] Step 1: Weigh 4.3403g SrCO 3 (AR), 0.1056g Eu 2 o 3 (purity>99.99%), put them in a zirconia ball mill jar after mixing, add zirconia balls and an appropriate amount of ball milling medium, the total amount of the sample should not exceed 2 / 3 of the ball mill jar, and ball mill for 3 hours on a planetary ball mill to make SrCO 3 and Eu 2 o 3 Mix well to form the primary mixture; put the ground primary mixture into a drying box and dry at 100°C for 4 hours; place the dried powder in an atmosphere furnace and fill it with N 2 / H 2 Mixed gas circulation, calcination temperature is 1000°C, calcination time is 6 hours; cool down with the furnace, take out the sample and grind it and sieve it with a 100-mesh standard inspection sieve, it is the mesophase silicate, and test the spectrum of the mesophase silicate ;

[0042] Step 2: Weigh 2.8056g Si 3 N 4 (purity>95%), then Si 3 N ...

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Abstract

The invention discloses metal silicon-based nitrogen oxide fluorescent powder and a preparation method thereof. The fluorescent powder is as shown in the general formula: M[1-x]Si2O2N2:xEu<2+>, wherein x is larger than 0 and smaller than 0.06, and M is one element or multiple elements selected from Ca, Sr and Ba. The fluorescent powder is wide in excitation range, stable in chemical and thermal properties and good in light-emitting effect; and the bathochromic shift of the peak of an emission spectrum appears along with the increment of the concentration of active ions. The invention also discloses a preparation method of the fluorescent powder, comprising the following steps of: generating silicate as an intermediate phase firstly, and then, generating a final product. The preparation method has the advantages that raw materials are simple, cost is low, operation is simple and easy, preparation temperature is low, equipment requirement is low and the like, and is capable of saving energy source and beneficial for large-scale industrial production; and the light-emitting performance of the fluorescent powder prepared by using the method is remarkably higher as compared with the traditional solid-phase one-step reaction method.

Description

technical field [0001] The invention belongs to the technical field of rare earth luminescent materials, and in particular relates to metal silicon-based nitrogen oxide fluorescent powder for warm white LEDs and a preparation method thereof. [0002] Background technique [0003] White LED has the advantages of high efficiency, energy saving, environmental protection, stable and reliable performance, and long service life. Its development will replace traditional lighting technology. Therefore, exploring new phosphors for white LEDs that can be excited by blue chips or ultraviolet light has become the current LED research hotspots. [0004] White LEDs are made of InGaN blue LED chips coated with Ce 3+ Activated yttrium aluminum garnet (Y 3 Al 5 o 12 , referred to as YAG: Ce 3+ ) composed of yellow phosphor powder, this white LED is a new type of solid-state lighting electric light source, which uses the blue light emitted by the blue LED chip to excite YAG: Ce 3+ Yell...

Claims

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Application Information

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IPC IPC(8): C09K11/59
Inventor 李海利张娜文波张偌雨卞先彬
Owner CHONGQING ACADEMY OF SCI & TECH
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