CN103215040A - Preparation method of calcium aluminosilicate blue phosphor powder for near-ultraviolet excited LED (Light Emitting Diode) - Google Patents

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

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CN103215040A
CN103215040A CN2013101451210A CN201310145121A CN103215040A CN 103215040 A CN103215040 A CN 103215040A CN 2013101451210 A CN2013101451210 A CN 2013101451210A CN 201310145121 A CN201310145121 A CN 201310145121A CN 103215040 A CN103215040 A CN 103215040A
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weighing
phosphor powder
preparation
calcium
solution
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朱达川
陆建平
陆俊娟
丁家伟
耿德英
孙健
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JIANGSU FUXIN ELECTRONIC LIGHTING SCIENCE AND TECHNOLOGY Co Ltd
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JIANGSU FUXIN ELECTRONIC LIGHTING SCIENCE AND TECHNOLOGY Co Ltd
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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

A kind of near ultraviolet excitated LED preparation method of calcium aluminosilicate blue colour fluorescent powder
Technical field
The invention belongs to the luminescent material technical field, be specifically related to the preparation method that a kind of near ultraviolet excitated LED uses the calcium aluminosilicate blue colour fluorescent powder.
Background technology
Along with global energy shortage, power tense and environmental pollution are serious, the green illumination product of exploitation and use energy-conserving and environment-protective has obtained whole world people's common recognition.LED is fast with its energy-saving and environmental protection, response speed, waterproof, characteristics such as shockproof, is regarded as one of high-tech industry of tool development prospect by countries in the world, is described as the green light source of 21 century.
At present, what blue-light excited type white light LEDs was the most frequently used on the market is that GaN chip and yellow fluorescent powder YAG:Ce3+ are packaged together, but glow color is owing to lack red light portion, and poor stability, light decay is serious, colour rendering index is low.In the last few years, along with the led chip continuous advancement in technology, the white light that adopts ultraviolet-near ultraviolet LED chip to excite three primary colors fluorescent powder to produce, colour stable, color developing good (Ra＞90) is considered to the developing direction of White-light LED illumination of new generation.
The preparation method of commercial fluorescent material, at present still based on high temperature solid-state method, as: CN101126024A, CN101525536A, CN101497791A, though being equipped with fluorescent material, this legal system has simple, the low cost and other advantages of technology, cause easily that crystal grain is thick, luminous efficiency is low but synthesis temperature height, calcination time are long, thing is assorted mutually, thereby cause that the use properties of fluorescent material and luminescent properties descend significantly.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of near ultraviolet excitated LED preparation method of calcium aluminosilicate blue colour fluorescent powder is provided.This kind method is by the suitable fluorescent material matrix component of design, adopt chemical coprecipitation in preparation matrix precursor, to finish the doping of rare earth ion, precursor is finished the reduction of decomposing with rare earth ion through once calcining in reducing atmosphere then, compare with the conventional high-temperature solid phase method, calcining temperature is low, the time is short, save the energy, and raw material is cheap and easy to get, technology is simple, is easy to suitability for industrialized production.
The near ultraviolet excitated white light LEDs that the present invention proposes with the chemical structural formula of calcium aluminosilicate blue phosphor is: Ca 1-xAl 2Si 2O 8: xEu 2+, 0＜x≤0.12.
The near ultraviolet excitated LED that the present invention proposes may further comprise the steps with the preparation method of calcium aluminosilicate blue colour fluorescent powder:
(1) presses chemical general formula Ca 1-xAl 2Si 2O 8: xEu 2+Take by weighing required calcium salt, aluminium salt, silicic acid and europium nitrate respectively; Take by weighing tensio-active agent and the fusing assistant of the 0.1wt%～1.5wt% of above medicine total mass more respectively;
(2) take by weighing precipitation agent, exceed fully to be settled out calcium, aluminium, europium ion, its amount for the 1.2-1.5 of theoretical reacting weight doubly, be configured to solution;
(3) with calcium salt, aluminium salt, nitrate, tensio-active agent wiring solution-forming, mix, slowly splash into precipitant solution, constantly stir simultaneously, fully carry out to precipitin reaction;
(4) with throw out washing, suction filtration, oven dry obtains presoma.
(5) presoma, fusing assistant, silicic acid are mixed, under reducing atmosphere, calcined 2-4 hour, obtain target product at 1150-1400 ℃.
Among the present invention, calcium salt described in the step (1) is analytically pure Ca (NO 3) 24H 2O or CaCl 26H 2O; Described aluminium salt is analytically pure Al (NO 3) 39H 2O or AlCl 3Described tensio-active agent is Sodium dodecylbenzene sulfonate or polyoxyethylene glycol; Described fusing assistant is H 3BO 3, MgF 2In a kind of.
Among the present invention, part is analytically pure NH described in the step (2) 4HCO 3, (NH 4) 2CO 3In a kind of.
Among the present invention, washings is distilled water or ethanol described in the step (4).
Among the present invention, reducing atmosphere is provided by the activated carbon powder combustion method described in the step (5), or uses nitrogen/hydrogen mixed gas.
Compared with prior art, the present invention has following beneficial effect:
1, the fluorescent material exciting light spectrum width prepared of the present invention can effectively be excited in 250～380nm wavelength region, is suitable as ultraviolet-near ultraviolet blue fluorescent powder for white-light LED.
2, the fluorescent material good crystallinity of the present invention's preparation, the luminous intensity height, and have good chemical stability and thermostability.
3, the fluorescent material prepared of the present invention adopts a calcining process, finishes doping simultaneously at the precursor pyrolysated, compares with the conventional high-temperature solid phase method, and calcining temperature is low, the time is short, and the production efficiency height is easy to suitability for industrialized production.
Description of drawings
Fig. 1 be a kind of near ultraviolet excitated white light LEDs provided by the present invention with the calcium aluminosilicate blue colour fluorescent powder process flow sheet;
Embodiment
Embodiment 1
Press chemical general formula Ca 0.985Al 2Si 2O 8: 0.015Eu 2+Take by weighing Ca (NO respectively 3) 2(A.R.) 0.985mol, Al (NO 3) 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.015mol; Take by weighing tensio-active agent Sodium dodecylbenzene sulfonate and the fusing assistant H of the 0.1wt% of above medicine total mass more respectively 3BO 3With the Ca (NO that takes by weighing 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing NH 4HCO 3(theoretical reacting weight 1.2 times), preparation NH 4HCO 3Solution slowly splashes into Ca (NO 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1300 ℃, and calcination time is 2.5 hours, promptly gets target product.
Embodiment 2
Press chemical general formula Ca 0.975Al 2Si 2O 8: 0.025Eu 2+Take by weighing CaCl respectively 2(A.R.) 0.975mol, AlCl 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.025mol; Take by weighing tensio-active agent Sodium dodecylbenzene sulfonate and the fusing assistant MgF of the 0.3wt% of above medicine total mass more respectively 2With the CaCl that takes by weighing 2, AlCl 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing NH 4HCO 3(theoretical reacting weight 1.3 times), preparation NH 4HCO 3Solution slowly splashes into CaCl 2, AlCl 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1400 ℃, and calcination time is 2 hours, promptly gets target product.
Embodiment 3
Press chemical general formula Ca 0.965Al 2Si 2O 8: 0.035Eu 2+Take by weighing Ca (NO respectively 3) 2(A.R.) 0.965mol, Al (NO 3) 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.035mol; Take by weighing surfactant polyethylene and the fusing assistant H of the 0.5wt% of above medicine total mass more respectively 3BO 3With the Ca (NO that takes by weighing 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing NH 4HCO 3(theoretical reacting weight 1.4 times), preparation NH 4HCO 3Solution slowly splashes into Ca (NO 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1150 ℃, and calcination time is 4 hours, promptly gets target product.
Embodiment 4
Press chemical general formula Ca 0.955Al 2Si 2O 8: 0.045Eu 2+Take by weighing CaCl respectively 2(A.R.) 0.955mol, AlCl 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.045mol; Take by weighing tensio-active agent Sodium dodecylbenzene sulfonate and the fusing assistant MgF of the 0.8wt% of above medicine total mass more respectively 2With the CaCl that takes by weighing 2, AlCl 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing NH 4HCO 3(theoretical reacting weight 1.4 times), preparation NH 4HCO 3Solution slowly splashes into CaCl 2, AlCl 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1200 ℃, and calcination time is 4 hours, promptly gets target product.
Embodiment 5
Press chemical general formula Ca 0.945Al 2Si 2O 8: 0.055Eu 2+Take by weighing Ca (NO respectively 3) 2(A.R.) 0.945mol, Al (NO 3) 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.055mol; Take by weighing tensio-active agent Sodium dodecylbenzene sulfonate and the fusing assistant H of the 1.0wt% of above medicine total mass more respectively 3BO 3With the Ca (NO that takes by weighing 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing NH 4HCO 3(theoretical reacting weight 1.5 times), preparation NH 4HCO 3Solution slowly splashes into Ca (NO 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1250 ℃, and calcination time is 3 hours, promptly gets target product.
Embodiment 6
Press chemical general formula Ca 0.935Al 2Si 2O 8: 0.065Eu 2+Take by weighing CaCl respectively 2(A.R.) 0.935mol, AlCl 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.065mol; Take by weighing surfactant polyethylene and the fusing assistant MgF of the 0.8wt% of above medicine total mass more respectively 2With the CaCl that takes by weighing 2, AlCl 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing NH 4HCO 3(theoretical reacting weight 1.4 times), preparation NH 4HCO 3Solution slowly splashes into CaCl 2, AlCl 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, calcine under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcining temperature is 1150 ℃, and calcination time is 4 hours, promptly gets target product.
Embodiment 7
Press chemical general formula Ca 0.915Al 2Si 2O 8: 0.095Eu 2+Take by weighing Ca (NO respectively 3) 2(A.R.) 0.915mol, Al (NO 3) 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.095mol; Take by weighing tensio-active agent Sodium dodecylbenzene sulfonate and the fusing assistant H of the 1.5wt% of above medicine total mass more respectively 3BO 3With the Ca (NO that takes by weighing 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing (NH 4) 2CO 3(theoretical reacting weight 1.3 times), preparation (NH 4) 2CO 3Solution slowly splashes into Ca (NO 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1200 ℃, and calcination time is 3.5 hours, promptly gets target product.
Embodiment 8
Press chemical general formula Ca 0.88Al 2Si 2O 8: 0.12Eu 2+Take by weighing Ca (NO respectively 3) 2(A.R.) 0.88mol, Al (NO 3) 39H 2O (A.R.) 2mol, H 2SiO 3(A.R.) 2mol and Eu (NO 3) 36H 2O (A.R.) 0.12mol; Take by weighing surfactant polyethylene and the fusing assistant MgF of the 1.3wt% of above medicine total mass more respectively 2With the Ca (NO that takes by weighing 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2O, tensio-active agent mix, and wiring solution-forming exceeds so that it fully dissolves, and takes by weighing (NH 4) 2CO 3(theoretical reacting weight 1.4 times), preparation (NH 4) 2CO 3Solution slowly splashes into Ca (NO 3) 2, Al (NO 3) 39H 2O, H 2SiO 3, Eu (NO 3) 36H 2In O, the tensio-active agent mixed solution, constantly stir, exceed fully to be settled out calcium, aluminium, europium ion; Suction filtration, washing, oven dry obtains precursor powder; After precursor powder and silicic acid, fusing assistant mixed, calcine under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcining temperature is 11500 ℃, and calcination time is 4 hours, promptly gets target product.

Claims (1)

1. a near ultraviolet excitated LED is with the preparation method of calcium aluminosilicate blue colour fluorescent powder, and its concrete steps are as follows:
(1) presses chemical general formula Ca 1-xAl 2Si 2O 8: xEu 2+, 0＜x≤0.12 takes by weighing required calcium salt, aluminium salt, silicic acid and europium nitrate respectively; Take by weighing tensio-active agent and the fusing assistant of the 0.1wt%～1.5wt% of above medicine total mass more respectively;
(2) take by weighing precipitation agent, exceed fully to be settled out calcium, aluminium, europium ion, its amount for the 1.2-1.5 of theoretical reacting weight doubly, be configured to solution;
(3) with calcium salt, aluminium salt, nitrate, tensio-active agent wiring solution-forming, mix, slowly splash into precipitant solution, constantly stir simultaneously, fully carry out to precipitin reaction;
(4) with throw out washing, suction filtration, oven dry obtains presoma;
(5) presoma, fusing assistant, silicic acid are mixed, under reducing atmosphere, calcined 2-4 hour, obtain target product at 1150-1400 ℃;
Among the present invention, calcium salt described in the step (1) is analytically pure Ca (NO 3) 24H 2O or CaCl 26H 2O; Described aluminium salt is analytically pure Al (NO 3) 39H 2O or AlCl 3Described tensio-active agent is Sodium dodecylbenzene sulfonate or polyoxyethylene glycol; Described fusing assistant is H 3BO 3, MgF 2In a kind of;
Among the present invention, part is analytically pure NH described in the step (2) 4HCO 3, (NH 4) 2CO 3In a kind of;
Among the present invention, washings is distilled water or ethanol described in the step (4);
Among the present invention, reducing atmosphere is provided by the activated carbon powder combustion method described in the step (5), or uses nitrogen/hydrogen mixed gas.
CN2013101451210A 2013-04-22 2013-04-22 Preparation method of calcium aluminosilicate blue phosphor powder for near-ultraviolet excited LED (Light Emitting Diode) Pending CN103215040A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106433628A (en) * 2016-08-30 2017-02-22 南昌大学 Eu-doped efficient-blue-light-emission aluminosilicate fluorescent material and preparation method
CN107674674A (en) * 2017-09-28 2018-02-09 苏州轻光材料科技有限公司 The preparation method of a kind of gold-tinted quantum dot and in white light LEDs application

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101735807A (en) * 2009-12-11 2010-06-16 四川大学 Aluminosilicate blue phosphor powder used for LEDs with near ultraviolet excitation and method for preparing same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101735807A (en) * 2009-12-11 2010-06-16 四川大学 Aluminosilicate blue phosphor powder used for LEDs with near ultraviolet excitation and method for preparing same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106433628A (en) * 2016-08-30 2017-02-22 南昌大学 Eu-doped efficient-blue-light-emission aluminosilicate fluorescent material and preparation method
CN106433628B (en) * 2016-08-30 2019-01-11 南昌大学 A kind of the aluminosilicate fluorescent material and preparation method of the high efficiency blue transmitting of Eu doping
CN107674674A (en) * 2017-09-28 2018-02-09 苏州轻光材料科技有限公司 The preparation method of a kind of gold-tinted quantum dot and in white light LEDs application

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Application publication date: 20130724