Preparation method of calcium aluminosilicate blue phosphor powder for near-ultraviolet excited LED (Light Emitting Diode)

A blue phosphor, calcium aluminosilicate technology, applied in luminescent materials, chemical instruments and methods, use of gas discharge lamps, etc., can solve the problem of the decline in performance and luminous performance of fluorescent powder, long calcination time, and low luminous efficiency and other problems, to achieve the effects of good chemical stability and thermal stability, good crystallinity and high luminous intensity

Inactive Publication Date: 2013-07-24
JIANGSU FUXIN ELECTRONICS LIGHTING TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] The preparation method of commercial fluorescent powder is still based on the high-temperature solid-phase method at present, such as: CN101126024A, CN101525536A, CN101497791A, although the preparation of fluorescent powder by this method has the advantages of simple pro...

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  • Preparation method of calcium aluminosilicate blue phosphor powder for near-ultraviolet excited LED (Light Emitting Diode)

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Experimental program
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Embodiment 1

[0023] According to chemical formula Ca 0.985 Al 2 Si 2 O 8 :0.015Eu 2+ Weigh Ca(NO 3 ) 2 (A.R.)0.985mol, Al(NO 3 ) 3 ·9H 2 O(A.R.)2mol, H 2 SiO 3 (A.R.)2mol and Eu(NO 3 ) 3 ·6H 2 O(A.R.) 0.015mol; then weigh 0.1wt% of the surfactant sodium dodecylbenzene sulfonate and flux H of the total mass of the above drugs 3 BO 3 ;Ca(NO 3 ) 2 , Al(NO 3 ) 3 ·9H 2 O, H 2 SiO 3 , Eu(NO 3 ) 3 ·6H 2 O. Mix the surfactants evenly and prepare a solution to make it fully dissolved. Weigh NH 4 HCO 3 (1.2 times the theoretical reaction volume), prepare NH 4 HCO 3 Solution, slowly drip Ca(NO 3 ) 2 , Al(NO 3 ) 3 ·9H 2 O, H 2 SiO 3 , Eu(NO 3 ) 3 ·6H 2 O. In the surfactant mixture, stir continuously to fully precipitate calcium, aluminum, and europium ions; filter, wash, and dry to obtain the precursor powder; mix the precursor powder, silicic acid, and flux evenly Afterwards, it is calcined in a reducing atmosphere provided by the combustion of activated carbon powder, the calcining temperature is 1300°C...

Embodiment 2

[0025] According to chemical formula Ca 0.975 Al 2 Si 2 O 8 :0.025Eu 2+ Weigh CaCl separately 2 (A.R.) 0.975mol, AlCl 3 ·9H 2 O(A.R.)2mol, H 2 SiO 3 (A.R.)2mol and Eu(NO 3 ) 3 ·6H 2 O(A.R.)0.025mol; then weigh 0.3wt% of the total mass of the above drugs, the surfactant sodium dodecylbenzene sulfonate and the flux MgF 2 ; CaCl to be weighed 2 , AlCl 3 ·9H 2 O, H 2 SiO 3 , Eu(NO 3 ) 3 ·6H 2 O. Mix the surfactants evenly and prepare a solution so that it can be fully dissolved. Weigh NH 4 HCO 3 (1.3 times the theoretical reaction volume), prepare NH 4 HCO 3 Solution, slowly drip into CaCl 2 , AlCl 3 ·9H 2 O, H 2 SiO 3 , Eu(NO 3 ) 3 ·6H 2 O. In the surfactant mixture, stir constantly to fully precipitate calcium, aluminum and europium ions; filter, wash, and dry to obtain the precursor powder; mix the precursor powder with silicic acid and flux evenly Afterwards, it is calcined in a reducing atmosphere provided by the combustion of activated carbon powder, the calcining temperature is...

Embodiment 3

[0027] According to chemical formula Ca 0.965 Al 2 Si 2 O 8 :0.035Eu 2+ Weigh Ca(NO 3 ) 2 (A.R.)0.965mol, Al(NO 3 ) 3 ·9H 2 O(A.R.)2mol, H 2 SiO 3 (A.R.)2mol and Eu(NO 3 ) 3 ·6H 2 O(A.R.) 0.035mol; then weigh 0.5wt% of the surfactant polyethylene glycol and flux H of the total mass of the above drugs 3 BO 3 ;Ca(NO 3 ) 2 , Al(NO 3 ) 3 ·9H 2 O, H 2 SiO 3 , Eu(NO 3 ) 3 ·6H 2 O. Mix the surfactants evenly and prepare a solution so that it can be fully dissolved. Weigh NH 4 HCO 3 (1.4 times the theoretical reaction volume), to prepare NH 4 HCO 3 Solution, slowly drip Ca(NO 3 ) 2 , Al(NO 3 ) 3 ·9H 2 O, H 2 SiO 3 , Eu(NO 3 ) 3 ·6H 2 O. In the surfactant mixture, stir continuously to fully precipitate calcium, aluminum and europium ions; filter, wash, and dry to obtain the precursor powder; mix the precursor powder, silicic acid, and flux evenly Afterwards, it is calcined in a reducing atmosphere provided by the combustion of activated carbon powder at a calcining temperature of 1150°C an...

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Abstract

The invention discloses a preparation method of calcium aluminosilicate blue phosphor powder for a near-ultraviolet excited white LED (Light Emitting Diode) and belongs to the preparation technology of rare earth phosphor powder. The chemical formula of the calcium aluminosilicate blue phosphor powder disclosed by the invention is as follows: Ca(1-x)Al2Si2O8:xEU2+, wherein x is greater than 0 and less than or equal to 0.12. The preparation method disclosed by the invention comprises the following specific steps of: respectively weighing required calcium salt, aluminium salt, silicic acid and europium nitrate according to a chemical general formula of Ca1-xAl2Si2O8; then respectively weighting a surfactant and a fluxing agent accounting for 0.1-1.5wt% of the total mass of the above medicines; weighing a sufficient quantity of a precipitant to prepare as a solution; preparing the calcium salt, the aluminium salt, nitrate and the surfactant as a solution, uniformly mixing and slowly dropping into the precipitant solution, simultaneously and continuously stirring till a precipitin reaction is completely processed; washing, filtering and drying precipitate to acquire a precursor; uniformly mixing the precursor, the fluxing agent and the silicic acid, and calcining for 2-4 hours at temperature of 1150-1400 DEG C to acquire a target product. The phosphor powder prepared by the method disclosed by the invention is wide excitation wavelength, high in luminous intensity and good in crystallinity, and is suitably used as the blue phosphor powder for the white LED.

Description

Technical field [0001] The invention belongs to the technical field of luminescent materials, and specifically relates to a preparation method of a near-ultraviolet excited calcium aluminosilicate blue phosphor for LEDs. Background technique [0002] With global energy shortages, power shortages and serious environmental pollution, the development and use of energy-saving and environmentally-friendly green lighting products has gained the consensus of people all over the world. LED is recognized as one of the most promising high-tech industries by countries all over the world for its energy saving, environmental protection, fast response speed, waterproof, shockproof and other characteristics, and is known as the green light source of the 21st century. [0003] At present, the most commonly used blue excitation white LED on the market is to encapsulate GaN chips and yellow phosphor YAG:Ce3+. However, due to the lack of red light, the light-emitting color has poor stability, severe ...

Claims

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Application Information

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IPC IPC(8): C09K11/80
CPCY02B20/181Y02B20/00
Inventor 朱达川陆建平陆俊娟丁家伟耿德英孙健
Owner JIANGSU FUXIN ELECTRONICS LIGHTING TECH
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