CN102703065A - Silicate green emitting phosphor powder for near ultraviolet excited light emitting diode (LED) - Google Patents

Silicate green emitting phosphor powder for near ultraviolet excited light emitting diode (LED) Download PDF

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Publication number
CN102703065A
CN102703065A CN201210215546XA CN201210215546A CN102703065A CN 102703065 A CN102703065 A CN 102703065A CN 201210215546X A CN201210215546X A CN 201210215546XA CN 201210215546 A CN201210215546 A CN 201210215546A CN 102703065 A CN102703065 A CN 102703065A
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near ultraviolet
phosphor powder
led
ball milling
weighing
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曹仕秀
彭玲玲
韩涛
程小耀
杨小琴
魏宁
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention relates to a synthesis method of silicate green emitting phosphor powder for a near ultraviolet excited light emitting diode (LED), which belongs to the preparation technology of rear earth phosphor powder. The chemical formula of the silicate is Ba1-xSiO3:xEu<2+>, wherein x is more than 0 and less than 0.1. The synthesis method of the silicate green emitting phosphor powder comprises following steps of measuring barium salt, silicic acid, europium nitrate and surface active agent and cosolvent with defined amount as required according to the chemical formula; adequately mixing the barium salt, the silicic acid, the europium nitrate, the surface active agent and ligand with defined amount, and then ball-milling, and adding a lubricant with defined amount in the ball milling process; filtering, washing and drying to obtain the precursor; and mixing the precursor with the cosolvent to be calcined under a reduction atmosphere to obtain the needed phosphor powder. The phosphor powder prepared by the method has the characteristics of wide laser excitation wavelength, high light emitting intensity, good crystallization and narrow distribution of granularity and is suitable for being used as the green emitting phosphor powder for the near ultraviolet excited white LED.

Description

A kind of near ultraviolet excitated LED uses silicate green fluorescent powder
Technical field
The invention belongs to the luminescent material technical field, be specifically related to a kind of near ultraviolet excitated LED and use silicate green fluorescent powder.
Background technology
White-light LED illumination is as a kind of novel solid light source, be described as the 4th generation green illumination light source.With life-span length, energy-saving and environmental protection, remarkable advantage such as volume is little, speed of response is fast, in illumination and demonstration field great application prospect is arranged, started one white light LEDs upsurge at global semiconductor and lighting field.
In recent years, people generally adopt near ultraviolet-ultraviolet (350～410nm) transmitting InGaN tube cores excite three primary colors fluorescent powder realizing white light LEDs, or add green and red fluorescence powder with blue-light LED chip, obtain the white light LEDs of high-color rendering, low colour temperature.LED fluorescent material adopts silicate as luminescent material matrix more; On the one hand because the silicate starting materials source is abundant, the preparation method is simple and flexibility is strong, crystalline structure stable; There is influence in the variation of chemical ingredients to the fluorescent material emmission spectrum; Composition through adjusting several materials or carry out codoped and realize that spectrographic selects because the silicate-base fluorescent RE powder exists effectively in the near-ultraviolet light zone absorbs, becomes the research emphasis of near ultraviolet excitated fluorescent material substrate material on the other hand.But existing silicate fluorescent powder is applicable to the less of used near ultraviolet LED, and the preparation method, is main with high temperature solid-state method mainly at present.Like CN101948689A, CN101948687A, wherein CN01029230A discloses a kind of oxynitride green emitting phosphor, produces the white light LEDs that high-color rendering hangs down colour temperature with nitride red fluorescent material Sr2Si5N8 coupling.That this method has is easy and simple to handle, technology simple, low cost and other advantages.But the high temperature solid-state method synthesis temperature is high, the calcining soaking time is long, and thing is assorted mutually and particle is thick, and pattern is irregular.Follow-up disintegrating process can cause declining to a great extent of light-emitting phosphor performance and use properties.The fluorescent material particle diameter narrowly distributing of combustion method patent such as CN101280189A, CN1730606A preparation, synthesis temperature is low, the energy-and time-economizing, but purity is low, luminescent properties is poor, has a large amount of gas to emit in the preparation process, is unfavorable for environment protection.
Therefore, simplicity of design is prone to row, preparation method cheaply, and research is fit to the LED that near ultraviolet efficiently excites and has vast market prospect with silicate green fluorescent powder.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of near ultraviolet excitated LED with silicate green fluorescent powder and preparation method thereof.This method is a raw material with barium salt, silicic acid and solid rare earth salt, part; Solid state reaction takes place in the room-temperature ball-milling process; Utilize the mechanical force (shearing force, surging force) that produces in the mechanical milling process can broken solid-phase reactant; Increase the specific surface area of reactant, improve reactant contact surface and speed of reaction, therefore improved the ratio of nucleation rate and growth rate; Prepare fine, uniform precursor, the precursor that reaction generates obtains even adulterated title product through washing, drying, thermolysis.
The near ultraviolet excitated LED that the present invention proposes may further comprise the steps with silicate green fluorescent powder and preparation method thereof:
(1) according to chemical formula Ba 1-xSiO 3: xEu 2+Take by weighing required barium salt, silicic acid and europium nitrate respectively; Take by weighing tensio-active agent and the fusing assistant of the 0.1wt%～0.2wt% of above medicine total mass more respectively;
(2) with the barium salt that takes by weighing, silicic acid, europium nitrate, tensio-active agent and an amount of part thorough mixing; The mol ratio 1:3 of reactant and part～6; Carry out ball milling then; Add lubricant during ball milling, the add-on of lubricant is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction;
(3) with above-mentioned product suction filtration, washing, oven dry obtains the precursor powder;
(4) precursor powder and solubility promoter are mixed after, under reducing atmosphere, calcine, calcining temperature is 1000 ℃～1300 ℃, calcination time is 2～5 hours, obtains title product.
Among the present invention, barium salt is Ba (NO described in the step (1) 3) 2, BaCO 3Or BaCl 22H 2O; Described tensio-active agent is X 2073 or polyoxyethylene glycol; Said fusing assistant is H 3BO 3, CaCl 2, Li 2CO 3In one or more.
Among the present invention, part is NH described in the step (2) 4HCO 3, (NH 4) 2CO 3, NH 3H 2A kind of among the O; Said lubricant is ethanol or acetone.
Among the present invention, reducing atmosphere is provided by the activated carbon powder combustion method described in the step (4), or uses nitrogen/hydrogen mixed gas.
Compared with prior art, the present invention has following beneficial effect:
1, the fluorescent material prepared of the present invention can effectively absorb the excitation wavelength in 300～410nm scope, is suitable as near ultraviolet (350～410nm) white light LEDs green emitting phosphors.
2, synthetizing phosphor powder of the present invention adopts a calcining process, accomplishes doping simultaneously at the precursor pyrolysated, compares with traditional high temperature solid-state method, and calcining temperature is low, and the time is short, and production efficiency is high.
3, the present invention adopts the mechanical force and chemical reaction method to prepare fluorescent material, good crystallinity, and particle is tiny, is evenly distributed, and technology is simple, and is easy to operate, good reproducibility.
4, the fluorescent material prepared of the present invention has good luminescent characteristic and stability.Four, description of drawings
Fig. 1 is the process flow sheet of a kind of near ultraviolet excitated LED provided by the invention with the preparation method of silicate green fluorescent powder;
Fig. 2 is green emitting phosphor Ba 0.95SiO 3: 0.05Eu 2+Supervisory wavelength is the excitation spectrum of 502nm;
Fig. 3 is green emitting phosphor Ba 0.95SiO 3: 0.05Eu 2+Supervisory wavelength is the emmission spectrum of 350nm.
Embodiment
Embodiment 1
Press chemical general formula Ba 0.98SiO 3: 0.02Eu 2+Take by weighing Ba (NO respectively 3) 2(A.R.) 0.98mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.02mol; Take by weighing tensio-active agent X 2073 and the fusing assistant H of the 0.1wt% of above medicine total mass more respectively 3BO 3With the Ba (NO that takes by weighing 3) 2(A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part NH 4HCO 3(reactant and part ratio are 1:3) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1000 ℃, and calcination time 2 hours promptly gets title product.
Embodiment 2
Press chemical general formula Ba 0.97SiO 3: 0.03Eu 2+Take by weighing Ba (NO respectively 3) 2(A.R.) 0.97mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.03mol; Take by weighing tensio-active agent X 2073 and the fusing assistant H of the 0.3wt% of above medicine total mass more respectively 3BO 3With the Ba (NO that takes by weighing 3) 2(A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part NH 4HCO 3(reactant and part ratio are 1:4) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1100 ℃, and calcination time 2 hours promptly gets title product.
Embodiment 3
Press chemical general formula Ba 0.96SiO 3: 0.04Eu 2+Take by weighing Ba (NO respectively 3) 2(A.R.) 0.96mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.04mol; Take by weighing tensio-active agent X 2073 and the fusing assistant H of the 0.5wt% of above medicine total mass more respectively 3BO 3With the Ba (NO that takes by weighing 3) 2(A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part NH 3H 2O (reactant and part ratio are 1:5) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcine, calcining temperature is 1300 ℃, and calcination time 3 hours promptly gets title product.
Embodiment 4
Press chemical general formula Ba 0.96SiO 3: 0.04Eu 2+Take by weighing BaCO respectively 3(A.R.) 0.96mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.04mol; Take by weighing surfactant polyethylene and the fusing assistant CaCl of the 0.8wt% of above medicine total mass more respectively 2With the BaCO that takes by weighing 3, H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part NH 3H 2O (reactant and part ratio are 1:5) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcine, calcining temperature is 1200 ℃, and calcination time 3 hours promptly gets title product.
Embodiment 5
Press chemical general formula Ba 0.95SiO 3: 0.05Eu 2+Take by weighing BaCO respectively 3(A.R.) 0.95mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.05mol; Take by weighing surfactant polyethylene and the fusing assistant CaCl of the 1wt% of above medicine total mass more respectively 2With the BaCO that takes by weighing 3(A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part (NH 4) 2CO 3(reactant and part ratio are 1:6) thorough mixing carries out ball milling then, adds lubricant ethanol during ball milling, and the alcoholic acid add-on is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcine, calcining temperature is 1250 ℃, and calcination time 3 hours promptly gets title product.
Embodiment 6
Press chemical general formula Ba 0.97SiO 3: 0.03Eu 2+Take by weighing BaCO respectively 3(A.R.) 0.97mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.03mol; Take by weighing tensio-active agent X 2073 and the fusing assistant Li of the 1.2wt% of above medicine total mass more respectively 2CO 3With the BaCO that takes by weighing 3, H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R), tensio-active agent and part NH 4HCO 3(reactant and part ratio are 1:4) thorough mixing carries out ball milling then, adds lubricant ethanol during ball milling, and the alcoholic acid add-on is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcine, calcining temperature is 1150 ℃, and calcination time 3 hours promptly gets title product.
Embodiment 7
Press chemical general formula Ba 0.94SiO 3: 0.06Eu 2+Take by weighing BaCl respectively 22H 2O (A.R.) 0.94mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.06mol; Take by weighing surfactant polyethylene and the fusing assistant Li of the 1.4wt% of above medicine total mass more respectively 2CO 3With the BaCl that takes by weighing 22H 2O (A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part (NH 4) 2CO 3(reactant and part ratio are 1:6) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, under nitrogen/hydrogen mixed gas provides reducing atmosphere, calcine, calcining temperature is 1050 ℃, and calcination time 5 hours promptly gets title product.
Embodiment 8
Press chemical general formula Ba 0.95SiO 3: 0.05Eu 2+Take by weighing BaCl respectively 22H 2O (A.R.) 0.95mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.05mol; Take by weighing surfactant polyethylene and the fusing assistant H of the 1.8wt% of above medicine total mass more respectively 3BO 3With the BaCl that takes by weighing 22H 2O (A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part (NH 4) 2CO 3(reactant and part ratio are 1:3) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1300 ℃, and calcination time 4 hours promptly gets title product.
Embodiment 9
Press chemical general formula Ba 0.96SiO 3: 0.04Eu 2+Take by weighing BaCl respectively 22H 2O (A.R.) 0.96mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.04mol; Take by weighing tensio-active agent X 2073 and the fusing assistant Li of the 2wt% of above medicine total mass more respectively 2CO 3With the BaCl that takes by weighing 22H 2O, H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part NH 4HCO 3(reactant and part ratio are 1:4) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1250 ℃, and calcination time 3 hours promptly gets title product.
Embodiment 10
Press chemical general formula Ba 0.94SiO 3: 0.06Eu 2+Take by weighing BaCl respectively 22H 2O (A.R.) 0.94mol, H 2SiO 3(A.R.) 1mol and Eu (NO 3) 36H 2O (A.R.) 0.06mol; Take by weighing surfactant polyethylene and the fusing assistant CaCl of the 1wt% of above medicine total mass more respectively 2With the BaCl that takes by weighing 22H 2O (A.R.), H 2SiO 3(A.R.), Eu (NO 3) 36H 2O (A.R.), tensio-active agent and part NH 3H 2O (reactant and part ratio are 1:5) thorough mixing carries out ball milling then, adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction; Suction filtration, washing, oven dry obtains the precursor powder; After precursor powder and fusing assistant mixed, provide under the reducing atmosphere in the activated carbon powder burning and to calcine, calcining temperature is 1200 ℃, and calcination time 3 hours promptly gets title product.

Claims (5)

1. a near ultraviolet excitated LED uses silicate green fluorescent powder, it is characterized in that material composition is europkium-activated silicate, and chemical structural formula is: Ba 1- x SiO 3: xEu 2+, wherein 0<x<0.1.
2. a kind of near ultraviolet excitated LED as claimed in claim 1 uses silicate green fluorescent powder, it is characterized in that concrete steps are following:
(1) according to chemical formula Ba 1- x SiO 3: xEu 2+Each element chemistry metering ratio, wherein 0<x<0.1, take by weighing corresponding barium salt, silicic acid and europium nitrate; Take by weighing tensio-active agent and the fusing assistant of 0.1wt% ~ 2 wt% of above medicine total mass more respectively;
(2) with the barium salt that takes by weighing, silicic acid and europium nitrate, tensio-active agent and appropriate amount of ligands thorough mixing; The mol ratio of reactant and part is 1:2 ~ 6; Carry out ball milling then; Add lubricant during ball milling, the add-on of lubricant is to be kept dispersion to exceed by the ball milling system, till reactant and part complete reaction;
(3) with above-mentioned product suction filtration, washing, oven dry obtains the precursor powder;
(4) precursor powder and solubility promoter are mixed after, calcining under reducing atmosphere, calcining temperature is 1000 ℃ ~ 1300 ℃, calcination time is 2 ~ 5 hours, promptly gets title product.
3. a kind of near ultraviolet excitated LED as claimed in claim 2 uses silicate green fluorescent powder, it is characterized in that barium salt is Ba (NO described in the step (1) 3) 2, BaCO 3Or BaCl 22H 2O; Said tensio-active agent is X 2073 or polyoxyethylene glycol; Said fusing assistant is H 3BO 3, CaCl 2, Li 2CO 3In one or more.
4. a kind of near ultraviolet excitated LED as claimed in claim 2 uses silicate green fluorescent powder, it is characterized in that part is NH described in the step (2) 4HCO 3, (NH 4) 2CO 3, NH 3H 2A kind of among the O; Said lubricant is ethanol or acetone.
5. a kind of near ultraviolet excitated LED as claimed in claim 2 uses silicate green fluorescent powder, it is characterized in that reducing atmosphere is provided by the activated carbon powder combustion method described in the step (4), or uses nitrogen/hydrogen mixed gas.
CN201210215546XA 2012-06-25 2012-06-25 Silicate green emitting phosphor powder for near ultraviolet excited light emitting diode (LED) Pending CN102703065A (en)

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Cited By (3)

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CN103468250A (en) * 2013-04-26 2013-12-25 四川大学 Preparation method of co-doped silicate green fluorescent powder used for LEDs
CN104774609A (en) * 2015-04-30 2015-07-15 中国科学院长春应用化学研究所 Long-afterglow luminescent material and preparation method thereof
CN105567224A (en) * 2016-03-02 2016-05-11 重庆文理学院 Synthetic method of borosilicate red nano fluorescent powder for LED

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103468250A (en) * 2013-04-26 2013-12-25 四川大学 Preparation method of co-doped silicate green fluorescent powder used for LEDs
CN103468250B (en) * 2013-04-26 2015-01-14 四川大学 Preparation method of co-doped silicate green fluorescent powder used for LEDs
CN104774609A (en) * 2015-04-30 2015-07-15 中国科学院长春应用化学研究所 Long-afterglow luminescent material and preparation method thereof
CN105567224A (en) * 2016-03-02 2016-05-11 重庆文理学院 Synthetic method of borosilicate red nano fluorescent powder for LED

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Application publication date: 20121003