CN105219378A - A kind of silicate blue fluorescent powder for white-light LED and preparation method thereof - Google Patents

A kind of silicate blue fluorescent powder for white-light LED and preparation method thereof Download PDF

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Publication number
CN105219378A
CN105219378A CN201510627389.7A CN201510627389A CN105219378A CN 105219378 A CN105219378 A CN 105219378A CN 201510627389 A CN201510627389 A CN 201510627389A CN 105219378 A CN105219378 A CN 105219378A
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fluorescent powder
white
present
blue fluorescent
fluorescent material
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CN105219378B (en
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余华
季振国
陈大钦
陈雷锋
钟家松
赵红挺
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Hangzhou Dianzi University
Hangzhou Electronic Science and Technology University
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Hangzhou Electronic Science and Technology University
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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 present invention relates to rare earth luminescent material technical field.A kind of silicate blue fluorescent powder for white-light LED, has following chemical representation: Na 2(Ca 0.5sr 0.5-x) (SiO 4): xEu 2+, wherein, x is 0.001 ~ 0.10.Advantage of the present invention is that sintering temperature is low, and synthesis technique is simple and raw material is cheap and easy to get.

Description

A kind of silicate blue fluorescent powder for white-light LED and preparation method thereof
Technical field
The present invention relates to rare earth luminescent material technical field, especially relate to a kind of silicate blue fluorescent powder for white-light LED and preparation method thereof.
Background technology
White light LEDs is a kind of solid-state semiconductor device converting electrical energy into white light, also known as semiconductor lighting, there is the plurality of advantages such as efficiency is high, volume is little, the life-span is long, safety, low voltage, energy-saving and environmental protection, being regarded as forth generation lighting source after incandescent light, luminescent lamp, high-voltage gas discharging light by people, is the main product in following illumination market.
There is various white light LEDs preparation method at present, wherein blue-light LED chip and yellow fluorescent material combine, blue-light LED chip and red and green fluorescent material combines, purple LED chip and fluorescent material with three basic colour combine these three kinds of methods low with price, prepare the main method simply becoming and prepare white light LEDs.It is that to study also be the most ripe method the earliest that blue-light LED chip and yellow fluorescent material combine, and the white light LEDs luminous efficiency of preparation is considerably beyond incandescent light, but colour rendering index is low, and colour temperature is high, can not use as interior lighting.In order to improve the color developing of white light LEDs, various countries scientist have developed blue-light LED chip and red, green fluorescent material combines and purple LED chip and red, green, blue fluorescent material with three basic colour combine other two kinds of methods realizing white light LEDs.
The emission wavelength of current InGaN chip moves near ultraviolet region, can provide higher excitation energy for fluorescent material, improves the light intensity of white light LEDs further.Because UV-light is invisible, the color of burst of ultraviolel white light LEDs can only be determined by fluorescent material, therefore colour stable, colour rendering index is high, uses near ultraviolet InGaN chip and blue, yellow fluorescent material or becomes the emphasis of current white light LEDs industry development with the scheme that three primary colors fluorescent powder combines to realize white light.Blue colour fluorescent powder is indispensable composition in the program.
LED blue colour fluorescent powder is mainly divided into several large system: sulphide fluorescent material, aluminate fluorescent powder, silicate fluorescent powder, phosphate phosphor and silica-based nitrogen (oxygen) compound fluorescent material.Sulfide blue colour fluorescent powder is as CaLaGa 3s 6o:Eu 2+.Aluminate blue fluorescent powder is as BaMgAl 10o 17: Eu 2+.Silicate blue fluorescent powder is as MSiO 4: Eu 2+(M=Ca, Sr, Ba), Y 2siO 5: Ce 3+, SrAl 2si 2o 8: Eu 2+, M 3mgSi 2o 8: Eu 2+(M=Ba, Sr) etc.Phosphate phosphor is as LiSrPO 4: Eu 2+, KSrPO 4: Eu 2+and SrMg 2(PO 4) 2: Eu 2+deng.Silica-based nitrogen (oxygen) compound blue colour fluorescent powder is as BaSi 2o 2n 2: Eu 2+, Ca 2si 5n 8: Ce 3+and Ba 2si 5n 8: Ce 3+deng.
Summary of the invention
The object of this invention is to provide a kind of sintering temperature low, simple silicate blue fluorescent powder for white-light LED of synthesis technique and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: a kind of silicate blue fluorescent powder for white-light LED, has following chemical representation: Na 2(Ca 0.5sr 0.5-x) (SiO 4): xEu 2+, wherein, x is 0.001 ~ 0.10.The preparation method of silicate blue fluorescent powder of the present invention comprises the steps: by chemical formula Na 2(Ca 0.5sr 0.5-x) (SiO 4): xEu 2+stoichiometric ratio take corresponding raw material, described raw material is respectively sodium carbonate, calcium carbonate, Strontium carbonate powder, silicon-dioxide and europium sesquioxide, and wherein x is 0.001 ~ 0.10; Be ground and obtain mixture; This mixture is loaded crucible, and in High Temperature Furnaces Heating Apparatus, sinter 3 ~ 7 hours under reducing atmosphere and 1250 ~ 1350 DEG C of conditions, rear cool to room temperature obtains described silicate blue fluorescent powder.
Further, reducing atmosphere of the present invention is nitrogen and hydrogen mixture or CO atmosphere.
Compared with prior art, the invention has the beneficial effects as follows: fluorescent material of the present invention is substrate material with silicate, has chemical stability and good thermal stability, raw material is inexpensive, be easy to get, the advantages such as sintering temperature is low.Compare sulfide blue colour fluorescent powder, Heat stability is good of the present invention.Compare aluminate blue fluorescent powder, preparation temperature of the present invention is lower than aluminate, and particle is thinner than aluminate, and luminosity is high, luminous efficiency is high and physical and chemical performance is stablized.Compare phosphate blue fluorescent powder, grain graininess of the present invention is even, Heat stability is good.Compare silica-based nitrogen (oxygen) compound blue colour fluorescent powder, sintering temperature of the present invention is low, and synthesis technique is simple and raw material is cheap and easy to get.
Accompanying drawing explanation
Fig. 1 is the fluorescent powder exciting light spectrogram of embodiment 1 provided by the invention preparation, supervisory wavelength 470nm;
Fig. 2 is the fluorescent powder utilizing emitted light spectrogram of embodiment 1 provided by the invention preparation, excitation wavelength 380nm;
Fig. 3 is the fluorescent powder XRD figure spectrum of embodiment 1 provided by the invention preparation.
Embodiment
Embodiment 1
According to Na 2(Ca 0.5sr 0.499-x) (SiO 4): 0.001Eu 2+take Na 2cO 3, CaCO 3, SrCO 3, SiO 2and Eu 2o 3, the mol ratio between them is 1:0.5:0.499:1:0.0005, and after abundant ground and mixed is even, place in corundum crucible, then put into High Temperature Furnaces Heating Apparatus 1350 DEG C of roastings 7 hours under CO atmosphere, rear cool to room temperature, obtains silicate blue fluorescent powder.
As can be seen from Figure 1, the fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet and violet region, and excitation peak is positioned near 380nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by ultraviolet and purple light chip.When the excitation wavelength of emmission spectrum is 380nm, as can be seen from Figure 2, the broadband blue light being emitted as divalent europium of the fluorescent material of the present embodiment is launched, and emission peak is positioned near 470nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet and purple light excited blue colour fluorescent powder.As can be seen from Figure 3, the fluorescent material XRD figure spectrum of the present embodiment shows the d value of product and the Na of relative intensity variation tendency and standard 2(Ca 0.5sr 0.499) (SiO 4) standard card (ICSD:33941) is consistent, illustrates that the fluorescent material purity that the present embodiment synthesizes is higher.
Embodiment 2
According to Na 2(Ca 0.5sr 0.499-x) (SiO 4): 0.005Eu 2+take Na 2cO 3, CaCO 3, SrCO 3, SiO 2and Eu 2o 3, the mol ratio between them is 1:0.5:0.495:1:0.0025, and after abundant ground and mixed is even, place in corundum crucible, then put into High Temperature Furnaces Heating Apparatus 1350 DEG C of roastings 5 hours under CO atmosphere, rear cool to room temperature, obtains silicate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet and violet region, and excitation peak is positioned near 380nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by ultraviolet and purple light chip.When the excitation wavelength of emmission spectrum is 380nm, the broadband blue light being emitted as divalent europium of the fluorescent material of the present embodiment is launched, and emission peak is positioned near 475nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet and purple light excited blue colour fluorescent powder.The fluorescent material XRD figure spectrum display d value of product of the present embodiment and the Na of relative intensity variation tendency and standard 2(Ca 0.5sr 0.499) (SiO 4) standard card (ICSD:33941) is consistent, illustrates that the fluorescent material purity that the present embodiment synthesizes is higher.
Embodiment 3
According to Na 2(Ca 0.5sr 0.49-x) (SiO 4): 0.01Eu 2+take Na 2cO 3, CaCO 3, SrCO 3, SiO 2and Eu 2o 3, the mol ratio between them is 1:0.5:0.49:1:0.005, and after abundant ground and mixed is even, place in corundum crucible, then put into High Temperature Furnaces Heating Apparatus 1250 DEG C of roastings 7 hours under CO atmosphere, rear cool to room temperature, obtains silicate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet and violet region, and excitation peak is positioned near 380nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by ultraviolet and purple light chip.When the excitation wavelength of emmission spectrum is 380nm, the broadband blue light being emitted as divalent europium of the fluorescent material of the present embodiment is launched, and emission peak is positioned near 477nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet and purple light excited blue colour fluorescent powder.The fluorescent material XRD figure spectrum display d value of product of the present embodiment and the Na of relative intensity variation tendency and standard 2(Ca 0.5sr 0.499) (SiO 4) standard card (ICSD:33941) is consistent, illustrates that the fluorescent material purity that the present embodiment synthesizes is higher.
Embodiment 4
According to Na 2(Ca 0.5sr 0.45-x) (SiO 4): 0.05Eu 2+take Na 2cO 3, CaCO 3, SrCO 3, SiO 2and Eu 2o 3, the mol ratio between them is 1:0.5:0.45:1:0.025, after abundant ground and mixed is even, places in corundum crucible, then puts into High Temperature Furnaces Heating Apparatus in 5%H 2+ 95%N 21300 DEG C of roastings 2 hours under the nitrogen and hydrogen mixture atmosphere of (volume ratio), rear cool to room temperature, obtains silicate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet and violet region, and excitation peak is positioned near 380nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by ultraviolet and purple light chip.When the excitation wavelength of emmission spectrum is 380nm, the broadband blue light being emitted as divalent europium of the fluorescent material of the present embodiment is launched, and emission peak is positioned near 480nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet and purple light excited blue colour fluorescent powder.The fluorescent material XRD figure spectrum display d value of product of the present embodiment and the Na of relative intensity variation tendency and standard 2(Ca 0.5sr 0.499) (SiO 4) standard card (ICSD:33941) is consistent, illustrates that the fluorescent material purity that the present embodiment synthesizes is higher.
Embodiment 5
According to Na 2(Ca 0.5sr 0.4) (SiO 4): 0.1Eu 2+take Na 2cO 3, CaCO 3, SrCO 3, SiO 2and Eu 2o 3, the mol ratio between them is 1:0.5:0.4:1:0.05, after abundant ground and mixed is even, places in corundum crucible, then puts into High Temperature Furnaces Heating Apparatus in 5%H 2+ 95%N 21250 DEG C of roastings 3 hours under the nitrogen and hydrogen mixture atmosphere of (volume ratio), rear cool to room temperature, obtains silicate blue fluorescent powder.
The fluorescent material excitation spectrum of the present embodiment is a wide range, covers ultraviolet and violet region, and excitation peak is positioned near 380nm, illustrates that the fluorescent material of the present embodiment effectively can be excited by ultraviolet and purple light chip.When the excitation wavelength of emmission spectrum is 380nm, the broadband blue light being emitted as divalent europium of the fluorescent material of the present embodiment is launched, and emission peak is positioned near 483nm, illustrates that the fluorescent material of the present embodiment is applicable to doing ultraviolet and purple light excited blue colour fluorescent powder.The fluorescent material XRD figure spectrum display d value of product of the present embodiment and the Na of relative intensity variation tendency and standard 2(Ca 0.5sr 0.499) (SiO 4) standard card (ICSD:33941) is consistent, illustrates that the fluorescent material purity that the present embodiment synthesizes is higher.

Claims (3)

1. a silicate blue fluorescent powder for white-light LED, is characterized in that, this fluorescent material has following chemical representation: Na 2(Ca 0.5sr 0.5-x) (SiO 4): xEu 2+, wherein, x is 0.001 ~ 0.10.
2. a preparation method for silicate blue fluorescent powder for white-light LED according to claim 1, is characterized in that comprising the steps: by chemical formula Na 2(Ca 0.5sr 0.5-x) (SiO 4): xEu 2+stoichiometric ratio take corresponding raw material, described raw material is respectively sodium carbonate, calcium carbonate, Strontium carbonate powder, silicon-dioxide and europium sesquioxide; Be ground and obtain mixture; This mixture is loaded crucible, and in High Temperature Furnaces Heating Apparatus, sinter 3 ~ 7 hours under reducing atmosphere and 1250 ~ 1350 DEG C of conditions, rear cool to room temperature obtains described silicate blue fluorescent powder.
3. the preparation method of silicate blue fluorescent powder for white-light LED as claimed in claim 2, is characterized in that: described reducing atmosphere is nitrogen and hydrogen mixture or CO atmosphere.
CN201510627389.7A 2015-09-28 2015-09-28 Silicate blue phosphor for white-light LEDs and preparation method thereof Active CN105219378B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116120922A (en) * 2023-02-17 2023-05-16 山东大学 Eu (Eu) 2+ Silicate doped fluorescent material and preparation method and application thereof

Citations (3)

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CN1880404A (en) * 2005-06-14 2006-12-20 大连路明发光科技股份有限公司 Red light-emitting phosphor powder excited by UV and blue light LED
WO2007029369A1 (en) * 2005-09-06 2007-03-15 Niigata University Fluorescent substance for light emitting diode
CN103059838A (en) * 2012-10-31 2013-04-24 苏州大学 Eu<2+> activated silicate yellow fluorescent powder as well as preparation method and application thereof

Patent Citations (3)

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CN1880404A (en) * 2005-06-14 2006-12-20 大连路明发光科技股份有限公司 Red light-emitting phosphor powder excited by UV and blue light LED
WO2007029369A1 (en) * 2005-09-06 2007-03-15 Niigata University Fluorescent substance for light emitting diode
CN103059838A (en) * 2012-10-31 2013-04-24 苏州大学 Eu<2+> activated silicate yellow fluorescent powder as well as preparation method and application thereof

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刘关喜等: "Na_2SrSiO_4:Ce~(3+),Tb~(3+),Yb~(3+)的制备及近红外量子剪裁发光性质", 《光谱实验室》 *

Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN116120922A (en) * 2023-02-17 2023-05-16 山东大学 Eu (Eu) 2+ Silicate doped fluorescent material and preparation method and application thereof
CN116120922B (en) * 2023-02-17 2024-01-30 山东大学 Eu (Eu) 2+ Silicate doped fluorescent material and preparation method and application thereof

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