CN1952039A - Sialon fluorescent powder for white light LED and electric light sources manufactured therefrom - Google Patents

Sialon fluorescent powder for white light LED and electric light sources manufactured therefrom Download PDF

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Publication number
CN1952039A
CN1952039A CNA2006101169864A CN200610116986A CN1952039A CN 1952039 A CN1952039 A CN 1952039A CN A2006101169864 A CNA2006101169864 A CN A2006101169864A CN 200610116986 A CN200610116986 A CN 200610116986A CN 1952039 A CN1952039 A CN 1952039A
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fluorescent material
preparation
white light
material according
led
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王宏志
李耀刚
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Donghua University
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Donghua 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
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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Abstract

The invention relates to a kind of fluorescence powder which can be used in white light LED. Its chemical formula is (M1-x/vNax) m/vSi12-m-nAlm+nOnN16-n: Rey. M stands for Ca, Li, Mg, Y, La, Nd, Lu ( one kind of the mentioned substance or various kinds of them); v stands for the value of M; Re stands for Eu, Ce, Dy, Tb, Pr, Sm, Y (one kind of the mentioned illuminating element or various kinds of them); 0.005<=x<=2.0;0.5<=m<=4.0;0<=n<=3.0;0.0005 <=y<=0.5. The producing process of the fluorescence powder is also disclosed in the invention. The fluorescence powder in the invention can react with the blue light LED to get the white light LED.

Description

A kind of sialon fluorescent powder of white light LEDs and made electric light source thereof of being used for
Technical field
The invention belongs to semiconductor applications, particularly relate to a kind of fluorescent material and preparation method thereof, and a kind of white light LED electric light source that contains this fluorescent material.
Background technology
The luminaire that white light emitting diode (LED) has than at present common usefulness has the longer life-span, littler volume, higher luminous efficiency, lower characteristics such as energy expenditure.Therefore, white light LEDs is considered to be in the alternative lighting source in some fields, the luminescent lamp of family expenses for example, backlight of liquid crystal indicator or billboard screen or the like.
It is by being the blue led and the yttrium aluminium garnet YAG of the InGaN base of 450nm in conjunction with wavelength that at present simple method is made white light LEDs: the Ce fluorescent material.This white light LEDs is undertaken by carrying out following step: at first, blue led emission blue light, the YAG:Ce fluorescent material absorbs a part of blue light and is converted into yellowish green fluorescence; Blue light and yellow-green fluorescence mix the formation white light then.But this white light only has the part of visible spectrum, causes lower colour rendering index (color rendering index).Simultaneously, the tone of this white light is colder, mainly is because the YAG:Ce fluorescent material contains less red composition.In order to obtain warm partially white light LEDs, YAG:Ce and another kind of red fluorescent material are mixed, but meanwhile, the luminous efficiency of the white light LEDs that obtains but descend, and influences practical effect.Illumination for the warm colour white light of realizing high-luminous-efficiency is necessary to research and develop a kind of novel fluorescent material, and it should have the characteristics that can effectively be excited by the wavelength of ultraviolet-blue light range and can launch yellow or orange-yellow fluorescence simultaneously.The silicate M2SiO4:Eu (M=Ca, Sr, Ba) of the europium doped of report is though can launch xanchromatic fluorescence at present, and this fluorescent material can not effectively be excited by blue led, and its poor heat stability, has influenced the luminous efficiency and the work-ing life of white light LEDs.
Summary of the invention
Technical problem to be solved
Technical problem to be solved by this invention provides a kind of sialon fluorescent powder of white light LEDs and made electric light source thereof of being used for, and is not enough and in the blue-light excited not high shortcoming of efficient down with the thermostability that overcomes existing yellow fluorescent powder.
Technical scheme
One of technical scheme of the present invention is to provide a kind of sialon fluorescent powder that is used for white light LEDs, (M 1-x/vNa x) M/vSi 12-m-nAl M+nO nN 16-n: Re y, wherein M is one or more among Ca, Li, Mg, Y, La, Nd, the Lu; V is the valence mumber of M; Re is one or more among rare earth luminous element Eu, Ce, Dy, Tb, Pr, Sm, the Yb; 0.005≤x≤2.0; 0.5≤m≤4.0; 0≤n≤3.0; 0.0005≤y≤0.5.
Two of technical scheme of the present invention is to provide a kind of method for preparing the described fluorescent material of claim 1, and steps in sequence comprises:
(1) with the oxide compound, nitride, fluorochemical or the salt that contain M, the nitride or the oxide compound that contain Re are raw material, and be according to the expressed proportioning raw materials batching of chemical formula, even through ground and mixed;
(2) mixture that obtains is carried out high-temperature calcination in high pressure nitrogen;
(3) with calcinate again through last handling process, promptly make fluorescent material of the present invention.
One of preferred version of the preparation method of above-mentioned fluorescent material is, in described step (2), the temperature of high-temperature calcination is 1500～2000 ℃, and calcination time is 0.5～60 hour.
Two of the preparation method's of above-mentioned fluorescent material preferred version is that the calcining of said step (2) repeatedly repeats.
Three of the preparation method's of above-mentioned fluorescent material preferred version is that in described step (2), nitrogen pressure is 1～20 normal atmosphere.
Four of the preparation method's of above-mentioned fluorescent material preferred version is that in described step (3), last handling process is followed successively by to be pulverized and washing impurity-removing.Said pulverizing is pulverized in mortar for manual, or utilizes comminution by gas stream, or utilizes ball mill pulverizing.Said washing impurity-removing steps in sequence comprises pickling, washing and drying.
The preparation method's of above-mentioned fluorescent material further preferred version is, said Acidwash solution is (sulfuric acid+hydrofluoric acid): deionized water=1: the mixed acid solution of (15～20) (volume ratio), sulfuric acid wherein: hydrofluoric acid=1: 2～2: 1, the pickling time is 0.5～2 hour; Said washing proceeds to the pH value for neutral; Said drying conditions is 80～120 ℃ and 2～12 hours.
Three of technical scheme of the present invention provides the described fluorescent material of a kind of claim 1 and combines the white light LED electric light source made from 430～480nm blue led.
Its implementation is: said white light LED electric light source is a light-emitting device, comprises the photodiode as luminous element, and the said fluor that contains the oxynitride sialon fluorescent powder of one of technical scheme.Wherein the wavelength that sends of photodiode comprises the blue light of 430～480nm, and the oxynitride sialon fluorescent powder absorbs the blue light that photodiode launches and launch gold-tinted or the orange-yellow fluorescence that wavelength is 550～610nm, the light of the two produces white light after mixing.
The said fluorescent material of one of technical solution of the present invention also can match with ultraviolet or near ultraviolet LED, and is green mixed mutually with red fluorescence powder with other again, the white light LED electric light source of preparation high color rendering index (CRI).
Beneficial effect
The present invention is by rare earth doped light-emitting element in heat-stable oxynitride Sialon, the method of partly replacing other metallic element with Na has been synthesized a kind of yellow or orange fluorescent powder that white light LED electric light source is made that can be used for to improve luminous intensity under high pressure nitrogen and high temperature.
White light LEDs provided by the invention can be excited by ultraviolet LED or blue-ray LED with oxynitride fluorescent powder, and thermally-stabilised height, luminescent properties excellence, luminous efficiency height, long service life.
Oxynitride fluorescent powder provided by the invention has the characteristics that can effectively be excited by the wavelength of ultraviolet-blue light range and can launch yellow or orange-yellow fluorescence simultaneously, has realized the illumination of the warm colour white light of high-luminous-efficiency.Overcome the silicate M of existing europium doped 2SiO 4: Eu (M=Ca, Sr, Ba) fluorescent material can not effectively be excited by blue led, and poor heat stability influences the luminous efficiency of white light LEDs and the shortcoming in work-ing life.
Description of drawings
Fig. 1 is the emmission spectrum of embodiment 12 white light LEDs.
Fig. 2 is emmission spectrum and the excitation spectrum of embodiment 1.
Fig. 3 is emmission spectrum and the excitation spectrum of embodiment 2.
Fig. 4 is emmission spectrum and the excitation spectrum of embodiment 3.
Fig. 5 is emmission spectrum and the excitation spectrum of embodiment 4.
Fig. 6 is emmission spectrum and the excitation spectrum of embodiment 5.
Fig. 7 is emmission spectrum and the excitation spectrum of embodiment 9.
Fig. 8 is emmission spectrum and the excitation spectrum of embodiment 11.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
The experimental technique of unreceipted actual conditions in the following example, usually according to the normal condition of bibliographical information, or the condition of advising according to manufacturer.
Embodiment 1:(Ca 0.75Na 0.5) 0.75Si 9Al 3O 1.5N 14.5: Eu 0.10Synthetic
CaCO 3: 8.0562 grams
Na 2CO 3: 3.1628 grams
Eu 2O 3: 1.5754 grams
Si 3N 4: 66.8364 grams
Al 2O 3: 4.0579 grams
The AlN:16.3113 gram
After in agate, grinding above-mentioned raw materials evenly, in the corundum crucible of packing into, be to calcine down in 1700 ℃ under 10 atmospheric nitrogen at pressure, calcination time 3 hours, take out the cooling back, utilizes ball mill pulverizing, sieves.(sulfuric acid+hydrofluoric acid): the mixed acid solution of deionized water=1: 15 (volume ratio), wherein sulfuric acid: hydrofluoric acid=1: 2 (volume ratio), the pickling time is 0.5 hour; Wash the pH value and approximate 7; Filter the powder obtain at last 120 ℃ of dryings 2 hours, obtain outward appearance and be xanchromatic fluorescent material, under the exciting of 254～500nm light, send the fluorescence of 580nm.
Embodiment 2:Li 0.5Na 0.5Si 9.5Al 2.5O 1.5N 14.5: Eu 0.05Synthetic
Li 2CO 3: 2.6739 grams
Na 2CO 3: 4.2369 grams
Eu 2O 3: 0.6754 gram
Si 3N 4: 70.8825 grams
Al 2O 3: 9.5132 grams
The AlN:12.0181 gram
After in agate, grinding above-mentioned raw materials evenly, pack in the corundum crucible, at pressure is in 1500 ℃ of calcinings down under 1 the atmospheric nitrogen, calcination time 60 hours, take out the cooling back, pulverizes in mortar by hand, sieve, (sulfuric acid+hydrofluoric acid): the mixed acid solution of deionized water=1: 18 (volume ratio), wherein sulfuric acid: hydrofluoric acid=1: 1 (volume ratio), the pickling time is 1 hour; Wash the pH value and approximate 7; Filter the powder obtain at last 80 ℃ of dryings 12 hours, obtain outward appearance and be xanchromatic fluorescent material, under the exciting of 254～500nm light, send the fluorescence of 568nm.
Embodiment 3:Na 2Si 8Al 4O 2N 14: Eu 0.05Synthetic
Na 2CO 3: 13.9748 grams
Eu 2O 3: 4.3672 grams
Si 3N 4: 56.6955 grams
Al 2O 3: 5.1523 grams
The AlN:20.7102 gram
After in agate, grinding above-mentioned raw materials evenly, pack in the corundum crucible, at pressure is to calcine down in 2000 ℃ under 20 atmospheric nitrogen, and calcination time 0.5 hour repeats calcining after the cooling, totally three times, take out, utilize comminution by gas stream to sieve, (sulfuric acid+hydrofluoric acid): the mixed acid solution of deionized water=1: 20 (volume ratio), sulfuric acid wherein: hydrofluoric acid=1: 2 (volume ratio), the pickling time is 1 hour; Wash the pH value and approximate 7; Filter the powder obtain at last 100 ℃ of dryings 8 hours, obtain outward appearance and be xanchromatic fluorescent material, under the exciting of 254～500nm light, send the fluorescence of 560nm.
Embodiment 4:(Y 0.667Na 0.5) 0.5Si 9.5Al 2.5O 1N 15: Eu 0.05Synthetic
Y 2O 3: 5.7698 grams
Na 2CO 3: 2.1011 grams
Eu 2O 3: 0.4744 gram
Si 3N 4: 70.3001 grams
Al 2O 3: 9.4350 grams
The AlN:11.9193 gram
After in agate, grinding above-mentioned raw materials evenly, pack in the corundum crucible, at pressure is in 1700 ℃ of calcinings down under 18 atmospheric nitrogen, calcination time 2 hours, crushing screening, (sulfuric acid+hydrofluoric acid): deionized water=1: the mixed acid solution of (15～20) (volume ratio) are taken out in the cooling back, sulfuric acid wherein: hydrofluoric acid=1: 1 (volume ratio), the pickling time is 1 hour; Wash the pH value and approximate 7; Filter the powder obtain at last 100 ℃ of dryings 10 hours, obtain outward appearance and be xanchromatic fluorescent material, under the exciting of 254～500nm light, send the fluorescence of 583nm.
Embodiment 5:Na 2Si 8Al 4O 2N 14: Ce 0.10Synthetic
Na 2CO 3: 12.1773 grams
CeO 2: 4.3734 grams
Si 3N 4: 57.3075 grams
Al 2O 3: 5.2079 grams
The AlN:20.9338 gram
After in agate, grinding above-mentioned raw materials evenly, pack in the corundum crucible, at pressure is in 1500 ℃ of calcinings down under 20 atmospheric nitrogen, calcination time 8 hours, crushing screening, (sulfuric acid+hydrofluoric acid): the mixed acid solution of deionized water=1: 20 (volume ratio) are taken out in the cooling back, sulfuric acid wherein: hydrofluoric acid=2: 1 (volume ratio), the pickling time is 2 hours; Wash the pH value and approximate 7; Filter the powder obtain at last 100 ℃ of dryings 10 hours, promptly obtain outward appearance and be xanchromatic fluorescent material, under the exciting of 400nm light, send the fluorescence of 480nm.
Embodiment 6-11: each embodiment chemical formula of pressing in the table 1 is formed and corresponding raw material, and preparation process is identical with embodiment 1, and the characteristics of luminescence that obtains fluorescent material sees Table 1.
The chemical formula and the characteristics of luminescence thereof of table 1 embodiment 6-13
Embodiment Chemical formula Excitation peak nm Fluorescence
6 (Lu 0.667Na 0.5) 0.5Si 9.5Al 2.5ON 15:Eu 0.05 412 Yellow, 584nm
7 (Ca 0.75Li 0.25Na 0.25) 0.75Si 9Al 3O 1.5N 14.5:Eu 0.10 425 Yellow, 574nm
8 (Ca 0.75Na 0.5) 0.75Si 9Al 3O 1.5N 14.5:Ce 0.10 386 Blueness, 500nm
9 (Ca 0.75Na 0.5) 0.75Si 9Al 3O 1.5N 14.5:Tb 0.10 254 Green, 545nm
10 (Ca 0.75Na 0.5) 0.75Si 9Al 3O 1.5N 14.5:Pr 0.05 254 Redness, 615nm
11 (Ca 0.75Na 0.5) 0.75Si 9Al 3O 1.5N 14.5:Sm 0.05 415 Redness, 602nm
Embodiment 12: the manufacturing of White LED light-emitting device
With weight ratio is fluorescent material and the Resins, epoxy that 2: 1 the mixed embodiment of the invention 1 makes, resulting mixture is coated on the chip of commercially available blue-ray LED (emission wavelength is 450nm), promptly obtaining white light LED electric light source after the oven dry of 150 ℃ and 0.5 hour, its emmission spectrum as shown in Figure 1.
Embodiment 13-22:
Fluorescent material in the fluorescent material alternate embodiment 12 that makes with embodiment of the invention 2-11 respectively, all the other methods is with embodiment 12, the preparation White LED light-emitting device.

Claims (10)

1. sialon fluorescent powder that is used for white light LEDs, its chemical formula is:
(M 1-x/vNa x) M/vSi 12-m-nAl M+nO nN 16-n: Re y, wherein M is one or more among Ca, Li, Mg, Y, La, Nd, the Lu; V is the valence mumber of M; Re is one or more among rare earth luminous element Eu, Ce, Dy, Tb, Pr, Sm, the Yb; 0.005≤x≤2.0; 0.5≤m≤4.0; 0≤n≤3.0; 0.0005≤y≤0.5.
2. method for preparing the described fluorescent material of claim 1, steps in sequence comprises:
(1) with the oxide compound, nitride, fluorochemical or the salt that contain M, the nitride or the oxide compound that contain Re are raw material, and be according to the expressed proportioning raw materials batching of chemical formula, even through ground and mixed;
(2) mixture that obtains is carried out high-temperature calcination in high pressure nitrogen;
(3) with calcinate again through last handling process, promptly make fluorescent material of the present invention.
3. the preparation method of fluorescent material according to claim 2, it is characterized in that: in described step (2), the temperature of high-temperature calcination is 1500～2000 ℃, and calcination time is 0.5～60 hour.
4. according to the preparation method of claim 2 or 3 described fluorescent material, it is characterized in that: the calcining of said step (2) repeatedly repeats.
5. the preparation method of fluorescent material according to claim 2, it is characterized in that: in described step (2), nitrogen pressure is 1～20 normal atmosphere.
6. the preparation method of fluorescent material according to claim 2 is characterized in that: in described step (3), last handling process is followed successively by to be pulverized and washing impurity-removing.
7. the preparation method of fluorescent material according to claim 6 is characterized in that: described pulverizing is pulverized in mortar for manual, or utilizes comminution by gas stream, or utilizes ball mill pulverizing.
8. the preparation method of fluorescent material according to claim 6, it is characterized in that: said washing impurity-removing steps in sequence comprises pickling, washing and drying.
9. the preparation method of fluorescent material according to claim 8, it is characterized in that: described Acidwash solution is (sulfuric acid+hydrofluoric acid): deionized water=1: the mixed acid solution of (15～20) (volume ratio), sulfuric acid wherein: hydrofluoric acid=1: 2～2: 1, the pickling time is 0.5～2 hour; Described washing proceeds to the pH value for neutral; Described drying conditions is 80～120 ℃ and 2～12 hours.
10. the described fluorescent material of claim 1 combines the white light LED electric light source made from 430～480nm blue led.
CNA2006101169864A 2006-10-11 2006-10-11 Sialon fluorescent powder for white light LED and electric light sources manufactured therefrom Pending CN1952039A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102082226A (en) * 2010-10-21 2011-06-01 罗维鸿 Natural light light-emitting diode (LED) and fluorescent powder thereof
CN102321473A (en) * 2011-02-16 2012-01-18 钟贤龙 Method for manufacturing fluorescent material with Mg-alpha-SiAlON as main crystal lattice
CN102433122A (en) * 2011-04-01 2012-05-02 奇美实业股份有限公司 Nitride phosphor, method for producing same, and light-emitting device
CN104080886A (en) * 2012-06-27 2014-10-01 独立行政法人物质·材料研究机构 Phosphor, method for producing same, light emitting device, and image display device
CN106221696A (en) * 2016-07-22 2016-12-14 中国科学院上海硅酸盐研究所 A kind of method improving rear-earth-doped Ca α Sialon oxynitride luminous intensity
CN104797684B (en) * 2012-11-13 2017-03-29 电化株式会社 Fluorophor, light-emitting component and lighting device

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102082226A (en) * 2010-10-21 2011-06-01 罗维鸿 Natural light light-emitting diode (LED) and fluorescent powder thereof
CN102082226B (en) * 2010-10-21 2012-09-05 罗维鸿 Natural light light-emitting diode (LED) and fluorescent powder thereof
CN102321473A (en) * 2011-02-16 2012-01-18 钟贤龙 Method for manufacturing fluorescent material with Mg-alpha-SiAlON as main crystal lattice
CN102433122A (en) * 2011-04-01 2012-05-02 奇美实业股份有限公司 Nitride phosphor, method for producing same, and light-emitting device
CN102433122B (en) * 2011-04-01 2014-03-19 奇美实业股份有限公司 Nitride phosphor, method for producing same, and light-emitting device
CN104080886A (en) * 2012-06-27 2014-10-01 独立行政法人物质·材料研究机构 Phosphor, method for producing same, light emitting device, and image display device
CN104080886B (en) * 2012-06-27 2017-05-24 国立研究开发法人物质·材料研究机构 Phosphor, method for producing same, light emitting device, and image display device
CN104797684B (en) * 2012-11-13 2017-03-29 电化株式会社 Fluorophor, light-emitting component and lighting device
CN106221696A (en) * 2016-07-22 2016-12-14 中国科学院上海硅酸盐研究所 A kind of method improving rear-earth-doped Ca α Sialon oxynitride luminous intensity
CN106221696B (en) * 2016-07-22 2018-08-28 中国科学院上海硅酸盐研究所 A method of improving rear-earth-doped Ca- α-Sialon oxynitride luminous intensities

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