Apatite-structure, wide-emission-band and green-light fluorescent powder for white-light LED, and preparation method thereof

An apatite and phosphor technology, which is applied in the field of apatite structure wide emission band green phosphor and its preparation, can solve problems such as low luminous efficiency, achieve high luminous intensity, high color purity, and cheap and easy raw materials the effect

Pending Publication Date: 2020-07-03
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Considering Ca 4 La 6 (SiO 4 ) 6 O:0.01Eu 2+ Apatite-type phosphors have the problem of low luminous efficiency

Method used

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  • Apatite-structure, wide-emission-band and green-light fluorescent powder for white-light LED, and preparation method thereof
  • Apatite-structure, wide-emission-band and green-light fluorescent powder for white-light LED, and preparation method thereof
  • Apatite-structure, wide-emission-band and green-light fluorescent powder for white-light LED, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Example 1: Preparation of Ca 3.99 La 6 (SiO 4 ) 6 O:0.01Eu 2+

[0023] Weigh CaCO in turn 3 (purity 99%) 1.0344g, La 2 o 3 (purity 99.99%) 2.5014g, SiO 2 (purity 99.99%) 0.9222g, Eu 2 o 3 (Purity 99.99%) 0.0045g. Put the above materials in a ball mill and grind them to 4 μm, mix well and put them in a high-purity corundum crucible, and put them into a high-temperature tube furnace, keep the heating rate in the furnace at 3°C / min, at 1350°C Incubate for 6 hours, then cool down to room temperature at a rate of 3°C / min. Maintain a volume fraction of 95% N throughout the furnace 2 with 5% H 2 mixed reducing atmosphere. The product cooled to room temperature was crushed, ball milled, and sieved with a 325-mesh sieve. Then use HNO with a concentration equivalent of 4N in sequence 3 Solution pickling, 4N NH 3 ·H 2 O solution alkaline washing, deionized water washing to neutral. Finally, the above-mentioned washed samples were centrifuged and layered, filtere...

example 2

[0024] Example 2: Preparation of Ca 3.99 La 6 (AlO 4 ) (SiO 4 ) 5 o 0.5 :0.01Eu 2+

[0025] Weigh CaCO in turn 3 (purity 99%) 1.0405g, La 2 o 3 (purity 99.99%) 2.5161g, Al 2 o 3 (purity 99.99%) 0.1312g, SiO 2 (purity 99.99%) 0.7730g, Eu 2 o 3 (Purity 99.99%) 0.0045g. Put the above materials in a ball mill and grind them to 4 μm, mix well and put them in a high-purity corundum crucible, and put them into a high-temperature tube furnace, keep the heating rate in the furnace at 3°C / min, at 1350°C Incubate for 6 hours, then cool down to room temperature at a rate of 3°C / min. Maintain a volume fraction of 95% N throughout the furnace 2 with 5%H 2 mixed reducing atmosphere. The product cooled to room temperature was crushed, ball milled, and sieved with a 325-mesh sieve. Then use HNO with a concentration equivalent of 4N in sequence 3 Solution pickling, 4N NH 3 ·H 2 O solution alkaline washing, deionized water washing to neutral. Finally, the above-mentioned w...

example 3

[0026] Example 3: Preparation of Ca 3.99 La 6 (AlO 4 ) 1.5 (SiO 4 ) 4.5 o 0.25 :0.01Eu 2+

[0027] Weigh CaCO in turn 3 (purity 99%) 1.0435g, La 2 o 3 (purity 99.99%) 2.5235g, Al 2 o 3 (purity 99.99%) 0.1973g, SiO 2 (purity 99.99%) 0.6978g, Eu 2 o 3 (Purity 99.99%) 0.0045g. Put the above materials in a ball mill and grind them to 4 μm, mix well and put them in a high-purity corundum crucible, and put them into a high-temperature tube furnace, keep the heating rate in the furnace at 3°C / min, at 1350°C Incubate for 6 hours, then cool down to room temperature at a rate of 3°C / min. Maintain a volume fraction of 95% N throughout the furnace 2 with 5% H 2 mixed reducing atmosphere. The product cooled to room temperature was crushed, ball milled, and sieved with a 325-mesh sieve. Then use HNO with a concentration equivalent of 4N in sequence 3 Solution pickling, 4N NH 3 ·H 2 O solution alkaline washing, deionized water washing to neutral. Finally, the above-me...

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Abstract

The invention discloses an apatite-structure, wide-emission-band and green-light fluorescent powder for a white-light LED, and a preparation method thereof. The general chemical formula of the fluorescent powder can be written into Ca4-yLa6(AlO4)x(SiO4)6-xO(1-0.5x): yEu<2+>, wherein x is more than or equal to 0 and less than or equal to 2, and ye is more than or equal to 0.01 and less than or equal to 0.06. The method comprises the following steps: weighing calcium carbonate, lanthanum oxide, aluminum oxide, silicon dioxide and europium oxide according to a certain molar ratio, uniformly ball-milling, and drying at normal temperature to obtain a raw material mixture; adding the raw material mixture into a crucible, putting the crucible into a high-temperature tubular furnace, and calciningfor 6 h in a reducing atmosphere (95% N2 + 5% H2) to obtain a blend; grinding and sieving the blend to obtain powder; sequentially carrying out acid washing, alkali washing and water washing on the sieved powder until the powder is washed to be neutral; and centrifugally layering, filtering and drying to obtain the green-light fluorescent powder for the white-light LED lamp. The green-light fluorescent powder for the white-light LED has the characteristics of high light-emitting brightness, high light-emitting efficiency, wide excitation wavelength range, wide emission wavelength range, capability of being well excited by an ultraviolet chip and the like.

Description

technical field [0001] The invention relates to the technical field of rare earth luminescent materials and energy saving and emission reduction, and specifically provides an apatite structure wide emission band green fluorescent powder for white LEDs and a preparation method thereof. Background technique [0002] In recent decades, rare earth luminescent materials have been widely used in lighting, electron optics, etc. White light-emitting diodes have excellent physical and chemical properties, such as environmental protection and long service life. In order to overcome the white light pc-LEDs (blue light excitation chip and YAG:Ce 3+ Due to the low color rendering index (CRI, Ra<80) and high relative color temperature (CCT, Tc>5500K) caused by the lack of red light components, many researchers tend to study white light that can be driven by near-ultraviolet chips Single-phase tunable emission phosphor powder for LED. [0003] As a good carrier of luminescent mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/80H01L33/50
CPCC09K11/7792H01L33/502H01L2933/0041Y02B20/00
Inventor 钱浩军宋开新徐明学范晨利刘兵徐军明高慧芳武军
Owner HANGZHOU DIANZI UNIV
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