CN102433114B - Fluorescent powder, and preparation method and application thereof - Google Patents

Fluorescent powder, and preparation method and application thereof Download PDF

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Publication number
CN102433114B
CN102433114B CN201110414626.3A CN201110414626A CN102433114B CN 102433114 B CN102433114 B CN 102433114B CN 201110414626 A CN201110414626 A CN 201110414626A CN 102433114 B CN102433114 B CN 102433114B
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fluorescent material
material according
fusing assistant
preparation
elements
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CN102433114A (en
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徐永华
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Beijing Jingchuangda Technology Co.,Ltd.
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BEIJING JINGCHUANGDA TECHNOLOGY CO LTD
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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 fluorescent powder, and a preparation method and application thereof. The chemical formula of the fluorescent powder is A[4-x]M[y]Si[6-z]N[10]O[w]:RE[x], wherein A is selected from one or more of Li, Mg, Ca, Sr, Ba, Be and Zn; M is selected from one or more of C, Ge, Sn, Ti, Hf, Mo, Zr, Al, W, Bi, B, Sc, Ga, In, Y and Gd; RE is active elements selected from one or more of Eu, Ce, Mn, Sm, La, Pr and Tb; and 0.002<=x<=0.5, 0<=y<6, 0<=z<6, and 0<=w<=1. The fluorescent powder provided by the invention has favorable development characteristic; and the independently used fluorescent powder can be packaged under the radiation of blue light LEDs to obtain a white light LED of which the development performance Ra is up to more than 85.

Description

A kind of fluorescent material and its preparation method and application
Technical field
The present invention relates to field of semiconductor illumination, be specifically related to a kind of fluorescent material and its preparation method and application.
Background technology
The features such as LED has efficiently, energy-conservation, safety, and the life-span is long, forth generation lighting system since being described as the use of the fire that continues.The implementation of LED white light has 2 kinds, and first kind of way is used alone redness, yellow and/or blue LED die, and second method is that ultraviolet or blue chip and fluorescent material are combined.Most economical in the market it is possible that adopt blue chip and yellow YAG phosphor to be combined realize LED illumination, particularly LED white-light illuminating, the method is applied for a patent (JP 8-198585) by Japanese Nichia company.But due to YAG fluorescent powder photoluminescent band narrow (band width is ~ about 120nm), lack red light portion, make the white light LEDs color developing prepared thus poor.For obtaining comparatively high-color rendering, method general at present uses blue chip and 2 kinds of fluorescent material, and namely yellow and red fluorescence powder is combined, or uses blue chip and 3 kinds of fluorescent material, and namely yellow, red and green emitting phosphor is combined realization.Latter two method mainly by making LED bands of a spectrum broaden, covers from blue light to green glow, and to gold-tinted and the part to ruddiness, the LED of realization has higher color developing.As mentioned above, at present for reaching higher color developing, multiple fluorescent material must be coordinated to use, due to the light efficiency of the fluorescent material of different substrates and kind and stability different, cause the complex process of allocating multiple fluorescent material in LED technique, the product good article rate obtained after encapsulation is low, and means of illumination easily occurs that look wafts.And along with the appearance of new packaging process, as fluorescent powder coating method, electrophoretic method and fluorescent material crystalline ceramics blade technolgy, make when applying above packaging process, the technique using multiple fluorescent material to realize white light LEDs becomes very complicated, even unfeasible.In the urgent need to a kind of new fluorescent material, when being used alone, higher color developing can be obtained.
Summary of the invention
The object of this invention is to provide a kind of fluorescent material obtained compared with high-color rendering.
Fluorescent material chemical formula of the present invention is A 4-xm ysi 6-Zn 10o w: RE x;
Wherein, A is selected from one or more in element Li, Mg, Ca, Sr, Ba, Be, Zn; M is selected from one or more in Elements C, Ge, Sn, Ti, Hf, Mo, Zr, Al, W, Bi, B, Sc, Ga, In, Y, Gd; RE is active element, is selected from one or more in Eu, Ce, Mn, Sm, La, Pr, Tb; X, y, z, w represent the numerical value of following scope respectively: 0.002≤x≤0.3,0≤y < 6,0≤z < 6,0≤w≤1.In addition, more than 90 % by mole one or more being selected from Elements C a, Sr, Ba of described A; Further, described A is selected from one or more in Elements C a, Sr, Ba.
The emission wavelength of phosphor material powder and general bandwidth can be regulated by regulating element ratio.
In addition, from the oxygen element that minimizing phosphor raw material is mixed into, and the stability aspect improving phosphor material powder is considered, described M is selected from one or more in Elements C, B, Al, Ga, Ge, Mo.
In addition, in order to the angle obtaining excellent emission wavelength, bands of a spectrum shape and luminous efficiency is considered, described RE is one or more in Eu, Ce, La; Further, described RE is one or more in Eu or Ce.
In addition, described x is 0.005≤x≤0.02; Described y is 0≤y≤3; Described z is 0≤z≤3.5.
Y is the content of element M in phosphor material powder, M is in the space structure of phosphor material powder, can regard that part replaces the position of Si element or N element as, simultaneously, the use of M element is of value to the oxygen level controlled in phosphor material powder, and improve luminescent properties and the stability of phosphor material powder, the preferred numerical range of y is: 0≤y≤3, as y > 3, there is the trend reduced in the brightness of phosphor material powder.
The present invention also provides a kind of method preparing described fluorescent material, and described method comprises the steps:
(1) compound containing A, M, RE and SiO is taken respectively by the stoichiometric ratio of fluorescent material 2or/and Si 4n 3mix;
(2) mixture is placed in crucible, carries out solid state reaction kinetics fluorescent material under anaerobic;
Wherein, the described compound containing A comprises: containing the oxide compound of A, nitride, carbonate or A simple substance;
The described compound containing M comprises: containing oxide compound or the nitride of M;
Compound containing RE comprises: containing the oxide compound of RE, nitride or halogenide.
In addition, described oxygen free condition is N 2atmosphere or reducing atmosphere; Described reducing atmosphere is the N of 5 ~ 20% 2/ H 2gas mixture, highly pure active charcoal reducing atmosphere or ammonia atmosphere.
In addition, the temperature of described solid state reaction is 1200 ~ 1800 DEG C, pressure is 0.1 ~ 1.0MPa, the time is 2 ~ 12 hours.In addition, in described step (1), add the fusing assistant of 0.05 ~ 10% of fluorescent material gross weight, described fusing assistant is halogenide, the NH of elements A 4cl or NH 4one or more in F; Further, the addition of described fusing assistant is 0.05 ~ 5% of fluorescent material gross weight, and described fusing assistant is SrF 2, NH 4cl or NH 4one or more in F.
Add fusing assistant, except there is the effect of adjustment material melting temperature, also charge balance is carried out to the composition of material, improve the stability of fluorescent material of the present invention.
The present invention also provides a kind of application of described fluorescent material, it is characterized in that, described fluorescent material is applied to LED.
Fluorescent material of the present invention can by ultraviolet, and near ultraviolet or blue-ray LED excite, and emission wavelength is between 530-710nm, and the peak width at half height of emission band is wider.When this fluorescent material is used for White-light LED illumination, comparatively high-color rendering can be obtained.
Accompanying drawing explanation
Fig. 1 is the emmission spectrum of embodiment 16 fluorescent material.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
According to the chemical formula Sr of fluorescent material 3.994si 5.989n 10o:Eu 0.005, take 0.133molSr 3n 2(38.74 grams), 0.183mol Si 3n 4(25.72 grams), 0.0499mol SiO 2, (3.00 grams) and 0.00025mol Eu 2o 3(0.088 gram), adds the SrF of fluorescent material weight 0.074% simultaneously 2(0.05 gram) fusing assistant, in the glove box of nitrogen protection ground and mixed evenly after, load in boron nitride crucible, proceed in High Temperature Furnaces Heating Apparatus.Be heated to 800 degree vacuumizing under state, now, pass into nitrogen, make high temperature furnace inner pressure be 0.5Mpa.Continue to be heated to 1550 degree, be incubated 1 hour, then with the speed of per minute 20 degree, temperature risen to 1800 degree, this temperature 2 hours.After cooling, take out product, carry out pulverizing, cleanup acid treatment, must Sr be consisted of 3.994si 6n 10o:Eu 0.005yellow fluorescent powder, in the present invention, the chemical structural formula of all fluorescent material is analyzed by quantitative elemental analysis and N, O and is determined.This phosphor emission wavelength is positioned at 580nm, and peak width at half height is 124nm.
Embodiment 2 ~ 3
Stoichiometric raw material Sr is taken respectively by fluorescent material chemical formula in table 1 embodiment 2,3 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the NH of 5% of fluorescent material gross weight 4cl is fusing assistant, and other are identical with the preparation method of embodiment 1, prepares the fluorescent material of 0.1mol respectively.
Embodiment 4 ~ 5
Stoichiometric raw material Sr is taken respectively by table 1 embodiment 4,5 fluorescent material chemical formula 3n 2, Eu 2o 3, Si 3n 4, SiO 2, meanwhile, add the SrF of 0.0001mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, prepare the fluorescent material of 0.1mol respectively.
Embodiment 6
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 6 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the SrF of 0.002mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 7
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 7 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the SrF of 0.001mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 8
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 8 3n 2, Ca 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the SrF of 0.0001mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 9
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 9 3n 2, Ca 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the NH of 0.05% of fluorescent material gross weight 4f is fusing assistant, and other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 10
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 10 3n 2, Ca 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the SrF of 0.0002mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 11 ~ 12
Stoichiometric raw materials of Ca is taken respectively by fluorescent material chemical formula in table 1 embodiment 11,12 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the NH of 0.1% of fluorescent material gross weight 4f is fusing assistant, and other are identical with the preparation method of embodiment 1, prepares the fluorescent material of 0.1mol respectively.
Embodiment 13
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 13 3n 2, Ba 3n 2, Si 3n 4, SiO 2, Eu 2o 3, meanwhile, add the SrF of 0.0001mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 14 ~ 17
Stoichiometric raw material Sr is taken respectively by fluorescent material chemical formula in table 1 embodiment 14 ~ 17 3n 2, Ca 3n 2, Ba 3n 2, Si 3n 4, SiO 2, Eu 2o 3and CeO 2, meanwhile, add the NH of 10% of fluorescent material gross weight 4cl is fusing assistant, and other are identical with the preparation method of embodiment 1, prepares the fluorescent material of 0.1mol respectively.
Embodiment 18
Stoichiometric raw material Sr is taken by fluorescent material chemical formula in table 1 embodiment 18 3n 2, Ba 3n 2, Si 3n 4, SiO 2, Eu 2o 3and CeO 2, meanwhile, add the SrF of 0.0002mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, the fluorescent material of preparation 0.1mol.
Embodiment 19 ~ 25
Stoichiometric raw material Sr is taken respectively by fluorescent material chemical formula in table 1 embodiment 19 ~ 25 3n 2, Ca 3n 2, AlN, BN, SiO 2, Si 3n 4, Eu 2o 3, meanwhile, add the NH of 8.5% of fluorescent material gross weight 4f is fusing assistant, and other are identical with the preparation method of embodiment 1, prepares the fluorescent material of 0.1mol respectively.
Embodiment 26 ~ 31
Stoichiometric raw material Sr is taken respectively by fluorescent material chemical formula in table 1 embodiment 26 ~ 31 3n 2, Ca 3n 2, BN, SiC, SiO 2, Si 3n 4, Eu 2o 3, meanwhile, add the NH of 7.2% of fluorescent material gross weight 4f is fusing assistant, and other are identical with the preparation method of embodiment 1, prepares the fluorescent material of 0.1mol respectively.
Embodiment 32 ~ 41
Stoichiometric raw material Sr is taken respectively by fluorescent material chemical formula in embodiment in table 1 32 ~ 41 3n 2, Ba 3n 2, Si 3n 4, AlN, BN, SiC, SiO 2, Eu 2o 3and CeO 2, meanwhile, add the SrF of 0.0002mol 2for fusing assistant, other are identical with the preparation method of embodiment 1, prepare the fluorescent material of 0.1mol respectively.
Table 1, fluorescent material and character thereof
Test example 1, application in White-light LED illumination
Take the fluorescent material of a certain amount of embodiment of the present invention 16,18,33,39, be dispersed in silicone resin, the mixture obtained after mixing deaeration process is coated on commercially available blue-light LED chip (emission wavelength is 457.5 ~ 460nm nm), heating 0.5 hour through 80 DEG C, after 150 DEG C of heating solidification in 2.5 hours, namely complete encapsulation.After the yellow light mix of the blue light that blue-ray LED is launched and phosphor emission, produce chromaticity coordinates, colour rendering index is as shown in table 2.
Table 2, fluorescent material application performance test
Application scheme Colour temperature Chromaticity coordinates Colour rendering index Ra
Blue-ray LED+embodiment 16 6500K 0.3205，0.3413 85
Blue-ray LED+embodiment 18 4500K 0.3336，0.3602 88
Blue-ray LED+embodiment 33 5500K 0.3305，0.3222 86
Blue-ray LED+embodiment 39 3300K 0.4200，0.4136 90
As can be seen from experimental example, fluorescent material of the present invention is applied in LED illumination has good color developing.

Claims (11)

1. a fluorescent material, is characterized in that, described fluorescent material chemical formula is A 4-xm ysi 6-Zn 10o w: RE x;
M is selected from one or more in Elements C, Ge, Sn, Ti, Hf, Mo, Zr, Al, W, Bi, B, Sc, Ga, In, Y, Gd; RE is active element, is selected from one or more in Eu, Ce, Mn, Sm, La, Pr, Tb; X, y, z, w represent the numerical value of following scope respectively: 0.002≤x≤0.3,0<y<6,0<z<6,0≤w≤1;
Wherein, described A is selected from one or more in Elements C a, Sr, Ba.
2. fluorescent material according to claim 1, is characterized in that, described M is selected from one or more in Elements C, B, Al, Ga, Ge, Mo.
3. fluorescent material according to claim 1, is characterized in that, described RE is one or more in Eu, Ce, La.
4. fluorescent material according to claim 3, is characterized in that, described RE is one or both in Eu or Ce.
5. fluorescent material according to claim 1, is characterized in that, described x is 0.005≤x≤0.02; Described y is 0<y≤3; Described z is 0<z≤3.5.
6., according to the arbitrary described fluorescent material of Claims 1 to 5, it is characterized in that, prepare by the following method:
(1) compound containing A, M, RE and SiO is taken respectively by the stoichiometric ratio of fluorescent material 2or/and Si 4n 3mix;
(2) mixture is placed in crucible, carries out solid state reaction kinetics fluorescent material under anaerobic;
Wherein, the described compound containing A comprises: containing the oxide compound of A, nitride, carbonate or A simple substance;
The described compound containing M comprises: containing oxide compound or the nitride of M;
Compound containing RE comprises: containing the oxide compound of RE, nitride or halogenide.
7. fluorescent material according to claim 6, is characterized in that, the temperature of described solid state reaction is 1200 ~ 1800 DEG C, pressure is 0.1 ~ 1.0MPa, the time is 2 ~ 12 hours.
8. fluorescent material according to claim 6, is characterized in that, described oxygen free condition is N 2atmosphere or reducing atmosphere; Described reducing atmosphere is the N of 5 ~ 20% 2/ H 2gas mixture, highly pure active charcoal reducing atmosphere or ammonia atmosphere.
9. fluorescent material according to claim 6, is characterized in that, in described step (1), add the fusing assistant of 0.05 ~ 10% of fluorescent material gross weight, described fusing assistant is halogenide, the NH of elements A 4cl or NH 4one or more in F.
10. fluorescent material according to claim 9, is characterized in that, the addition of described fusing assistant is 0.05 ~ 5% of fluorescent material gross weight, and described fusing assistant is SrF 2, NH 4cl or NH 4one or more in F.
The application of the arbitrary described fluorescent material of 11. claim 1 ~ 10, it is characterized in that, described fluorescent material is applied to LED.
CN201110414626.3A 2011-12-13 2011-12-13 Fluorescent powder, and preparation method and application thereof Expired - Fee Related CN102433114B (en)

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US8663502B2 (en) 2011-12-30 2014-03-04 Intematix Corporation Red-emitting nitride-based phosphors
KR101641378B1 (en) 2011-12-30 2016-07-20 인터매틱스 코포레이션 Nitride phosphors with interstitial cations for charge balance
CN102660268B (en) * 2012-05-11 2014-11-19 北京晶创达科技有限公司 Method for preparing nitride phosphor by using oxides as raw materials, and nitride phosphor
US8597545B1 (en) * 2012-07-18 2013-12-03 Intematix Corporation Red-emitting nitride-based calcium-stabilized phosphors
WO2014094975A1 (en) * 2012-12-21 2014-06-26 Merck Patent Gmbh Luminescent substances
CN104232087A (en) * 2014-08-11 2014-12-24 北京大学工学院包头研究院 Fluorescent material and preparation method and application thereof
TWI629339B (en) * 2017-06-16 2018-07-11 信源陶磁股份有限公司 Method for manufacturing nitride phosphor
CN110234736A (en) * 2017-11-20 2019-09-13 有研稀土新材料股份有限公司 A kind of fluorescent material and its made light emitting device

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