CN101824320A - Red fluorescent powder, preparation method and application thereof - Google Patents
Red fluorescent powder, preparation method and application thereof Download PDFInfo
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- CN101824320A CN101824320A CN201010176649A CN201010176649A CN101824320A CN 101824320 A CN101824320 A CN 101824320A CN 201010176649 A CN201010176649 A CN 201010176649A CN 201010176649 A CN201010176649 A CN 201010176649A CN 101824320 A CN101824320 A CN 101824320A
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Abstract
The invention discloses red fluorescent powder, a preparation method and application thereof, and belongs to the field of a fluorescent material. The chemical formula of the fluorescent powder is Ln2-xM2O7: xEu, wherein the Ln is one or combination of La, Gd and Y; M is one or combination of Ti, Zr, and Hf; Eu is a luminescence centre; doping is performed at Ln position; and the doping value of the Eu, namely x is equal to 0.02 to 1.0. The red fluorescent powder emits the fluorescence with the wave length of between 570 to 640nm after being excited by a blue light chip (455 to 465nm) or a near ultraviolet chip (380 to 395nm), and the wave length of the red luminescence is between 600 and 620nm. The red fluorescent powder can be used for a white LED and relevant displaying and lighting devices; and the red fluorescent powder has the advantages of simple preparation process, stable chemical property and excellent lighting property, and is the ideal fluorescent powder for the white LED.
Description
Technical field
The present invention belongs to the fluorescent material field, is specifically related to a kind of red fluorescence powder and its production and application.
Background technology
White light LEDs be after incandescent light, fluorescent lamp and electricity-saving lamp the 4th generation lighting electric light source, be called as the 21 century green light source, have environmental protection, overlong service life, energy-efficient, anti-adverse environment, simple in structure, volume is little, in light weight, response is fast, operating voltage is low and the good characteristics of security.It is trend of the times that the LED solid state light emitter substitutes the traditional lighting light source.
The mode that present white light LEDs sends white light mainly is to utilize the fluorescent material transformation approach.Business-like white light LEDs is that the InGaN tube core of emission blue streak (460nm) is formed with the YAG:Ce that launches gold-tinted.This mode technology is simple, and cost is lower, exists that color developing is poor, colour temperature is higher, lacks the shortcoming of red composition.Therefore, utilize this scheme to realize low colour temperature, Ra＞80 high color rendering index (CRI)s that 5000K is following, the warm white LED of high brightness is difficult, needs to add and can be improved performance by blue-light excited red fluorescence powder.Research and development can be excited by blue light is more effective, and the fluorescent material difficulty that photon conversion efficiency is higher is bigger.The photochromic meeting of LED becomes softer or bright-coloured, to adapt to different application needs, fluorescent material of all kinds all is widely used in white light and color LED field, but the application on color LED is also at the early-stage, need further carry out deep research and development.
The commercial red fluorescence powder that white light LEDs is used is confined to nitride, oxynitride and sulfide base material, has complicated, the characteristics such as cost is higher, military service poor stability of preparation.Even the YAG:Ce bloom has 20% luminous intensity decay under 80 ℃.Exploitation has the novel high-performance red LED fluorescent material that good luminous characteristic, chemical property are stable, cost is low, and is extremely urgent.
The outstanding substrate material of new fluorescent material is most important, must satisfy have good chemical stability, suitable energy gap and crystalline structure and low production cost.In sum, the LED that seeks good substrate material and then preparation luminescent properties excellence has great science and realistic meaning with fluorescent material.
Summary of the invention
The present invention proposes a kind of red fluorescence powder material Ln that is used for White-light LED illumination of being excited by Lan Se or near ultraviolet photodiode of can be used for
2M
2O
7: Eu (Ln=La, Gd, Y; M=Ti, Zr, Hf) and preparation method thereof.
Technical scheme of the present invention is:
The red fluorescence powder that a kind of LED excites, the chemical formula of this material can be expressed as Ln
2-xM
2O
7: xEu, and meet following condition: Ln be a kind of of La, Gd, Y or the combination, M be a kind of of Ti, Zr, Hf or the combination, wherein, Ln=La
2-x-y-zGd
yY
z(0≤y+z≤2-x, x are the doping of Eu) and M=Ti
2-x-yZr
xHf
y(0≤x+y≤2); Eu is a luminescence center, mixes to be positioned at the Ln position, doping value x=0.02-1.0, best x scope 0.3-0.5.The novel red luminescent material that this LED excites excites down at blue streak chip (455-465nm) or near-ultraviolet light chip (380-395nm), launches to be the fluorescence between the 570-640nm, and red fluorescence is between the 600-620nm.
The red fluorescence powder Ln that LED excites
2-xM
2O
7: xEu (Ln=La, Gd, Y; M=Ti, Zr, Hf) the preparation method adopt solid state reaction.At first press Ln
2-xM
2O
7: xEu chemical constitution proportioning selects for use an amount of raw material to prepare burden, and takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in corundum crucible or other container, carry out pre-burning in stove, temperature is 500～1000 ℃, and the time is 0～48h; The gained powder grinds the back and fires once more at 800～1500 ℃, and the reaction times is 12～96h, and this process can repeat; Prepared fluorescent powder ball milling, refinement and screening promptly obtain red fluorescence material.
The raw material that contains Ln and Eu that the present invention adopts is oxide compound, metal-powder, nitrate, acetate; The raw material that contains M is oxide compound, metal-powder, oxygen vitriol.
Innovation part of the present invention is Ln
2M
2O
7Material is by rare earth Eu
3+Mix to obtain the high brightness ruddiness that excites by blue look LED, can be in the doping content of Ln position up to 40mol%, and do not cause fluorescent quenching, doping content is considerably beyond common fluorescent material optimum value (being usually less than 5～10%).The matrix of this fluorescent material has the above band gap of 3eV, and overall fluorescent powder table color is white, presents redness under blue streak excites, and is very stable under concentrated acid, can overcome the YAG:Ce bloom has decay under high-temperature (50-80 ℃) characteristic.
Material of the present invention can be used for white light LEDs and be correlated with demonstration, illuminating device.Mentality of designing uniqueness of the present invention, raw material is cheap and easy to get, and preparation technology is simple, and the chemical property of material is stable, and the luminescent properties excellence is an ideal phosphor for white light LED candidate material.
Description of drawings
La among Fig. 1: the embodiment 1
1.6Ti
2O
7: the powder X-ray RD spectrum of 0.4Eu sample;
La among Fig. 2: the embodiment 1
1.6Ti
2O
7: the excitation spectrum of 0.4Eu sample;
La among Fig. 3: the embodiment 1
1.6Ti
2O
7: the emmission spectrum of 0.4Eu sample.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail:
Embodiment 1,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to La
1.6Ti
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening, promptly obtain the red fluorescence material (XRD sees Fig. 1) of pure phase, the excitation spectrum of sample is seen Fig. 2, the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 73000 (see figure 3)s, and the fluorescent emission intensity at the 617nm place under the 390nm near ultraviolet excitation reaches 36000.
Embodiment 2,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to La
1.6Ti
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 500 ℃, and the time is 48h; Pre-burning gained powder grinds the back and fires once more at 1000 ℃, and the reaction times is 12h; Pre-burning gained powder grinds the back and fires once more at 1500 ℃, and the reaction times is 12h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 80000.
Embodiment 3,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to La
1.6Ti
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, without pre-burning, fire at 1500 ℃ in stove, the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 69000.
Embodiment 4,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to La
1.98Ti
2O
7: the stoichiometric ratio of 0.02Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 13000.
Embodiment 5,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to LaTi
2O
7: the stoichiometric ratio of Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 63000.
Embodiment 6,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to La
1.7Ti
2O
7: the stoichiometric ratio of 0.3Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 72000.
Embodiment 7,
At first with raw material La
2O
3, TiO
2, Eu
2O
3According to La
1.5Ti
2O
7: the stoichiometric ratio of 0.5Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 71000.
Embodiment 8,
At first with raw material Gd
2O
3, TiO
2, Eu
2O
3According to Gd
1.6Ti
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 75000.
Embodiment 9,
At first with raw material La
2O
3, Y
2O
3, TiO
2, Eu
2O
3According to La
0.6YTi
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 85000.
At first with raw material La
2O
3, Y
2O
3, Gd
2O
3, TiO
2, Eu
2O
3According to La
0.6Y
0.5Gd
0.5Ti
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 82000.
Embodiment 11,
At first with raw material La (Ac)
3, ZrO
2, Eu
2O
3According to La
1.6Zr
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 24h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 73000.
Embodiment 12,
At first with raw material La
2O
3, ZrO
2, Eu
2O
3According to La
1.6Zr
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in corundum crucible or other container, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 800 ℃, and the reaction times is 96h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 73000.
Embodiment 13,
At first with raw material La
2O
3, TiO
2, ZrO
2, Eu
2O
3According to La
1.6TiZrO
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1300 ℃, and the reaction times is 48h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 85000.
Embodiment 14,
At first with raw material Gd (NO
3)
36H
2O, Y (NO
3)
36H
2O, TiOSO
4, ZrOSO
4, Eu (NO
3)
36H
2O is according to Gd
0.1Y
1.5TiZrO
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1300 ℃, and the reaction times is 48h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, reach 86500 in 617nm place emitted fluorescence emissive porwer under the 465nm blue streak excites.
Embodiment 15,
At first with raw material La, Ti, Eu
2O
3According to La
1.6Ti
2O
7: the stoichiometric ratio of 0.4Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 900 ℃, and the time is 48h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 96h; Prepared fluorescent powder ball milling, refinement and screening promptly obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at the 617nm place under the 465nm blue streak excites reaches 71000.
More than by specific embodiment red fluorescence powder provided by the present invention and its production and application has been described, it will be understood by those of skill in the art that in the scope that does not break away from essence of the present invention, can make certain conversion or modification to the present invention; Be not limited to disclosed content among the embodiment.
Claims (7)
1. a fluorescent material is characterized in that, the chemical formula of this fluorescent material is expressed as Ln
2-xM
2O
7: xEu, and meet following condition:
1) Ln is a kind of of La, Gd, Y or combination, and M is a kind of of Ti, Zr, Hf or combination;
2) Eu is a luminescence center, mixes to be positioned at Ln position, the doping value x=0.02-1.0 of Eu.
2. fluorescent material as claimed in claim 1 is characterized in that Ln=La
2-x-y-zGd
yY
z, 0≤y+z≤2-x wherein.
3. fluorescent material as claimed in claim 1 or 2 is characterized in that M=Ti
2-x-yZr
xHf
y, 0≤x+y≤2 wherein.
4. one kind prepares the method for fluorescent material according to claim 1, it is characterized in that, adopts the solid state reaction preparation, and concrete steps are as follows:
A) press Ln
2-xM
2O
7: xEu chemical constitution proportioning selects for use an amount of raw material to prepare burden, and takes ball mill mixing, makes batch mixing refinement and fully mixed;
B) batch mixing behind the ball milling is packed in corundum crucible or other container, carry out pre-burning in stove, temperature is 500～1000 ℃, and the time is 0～48h; The gained powder grinds the back and fires once more at 800～1500 ℃, and the reaction times is 12～96h; Last process can repeat.
C) prepared fluorescent powder ball milling, refinement and screening.
5. method as claimed in claim 4 is characterized in that, the raw material that contains Ln and Eu is oxide compound, metal-powder, nitrate or acetate.
6. as claim 4 or 5 described methods, it is characterized in that the raw material that contains M is oxide compound, metal-powder or oxygen vitriol.
7. the application of the described fluorescent material of claim 1 in LED blue streak chip or near-ultraviolet light chip.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624321A (en) * | 2017-11-21 | 2018-10-09 | 杭州显庆科技有限公司 | One kind Lu containing lithium2Zr2O7System phosphor |
| CN108913141A (en) * | 2018-08-01 | 2018-11-30 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorescent material and its preparation and application |
| WO2022187349A1 (en) * | 2021-03-02 | 2022-09-09 | The Regents Of The University Of California | Combinatory therapy for preventing, inhibiting, treating, or reducing aneurysms |
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| CN101629079A (en) * | 2009-08-17 | 2010-01-20 | 浙江理工大学 | Method for preparing green luminescent material of yttrium zirconate doped with terbium |
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| CN101016455A (en) * | 2007-02-06 | 2007-08-15 | 浙江理工大学 | Method of preparing composite europium samarium stannate nano fluorescent powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624321A (en) * | 2017-11-21 | 2018-10-09 | 杭州显庆科技有限公司 | One kind Lu containing lithium2Zr2O7System phosphor |
| CN108913141A (en) * | 2018-08-01 | 2018-11-30 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorescent material and its preparation and application |
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| CN108913141B (en) * | 2018-08-01 | 2021-04-20 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorescent material, preparation and application thereof |
| WO2022187349A1 (en) * | 2021-03-02 | 2022-09-09 | The Regents Of The University Of California | Combinatory therapy for preventing, inhibiting, treating, or reducing aneurysms |
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Application publication date: 20100908 |