CN102277172A - Rare earth luminescent material and its preparation method - Google Patents

Rare earth luminescent material and its preparation method Download PDF

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CN102277172A
CN102277172A CN2010102022609A CN201010202260A CN102277172A CN 102277172 A CN102277172 A CN 102277172A CN 2010102022609 A CN2010102022609 A CN 2010102022609A CN 201010202260 A CN201010202260 A CN 201010202260A CN 102277172 A CN102277172 A CN 102277172A
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rare earth
luminescent material
earth luminescent
preparation
metal nanoparticle
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CN102277172B (en
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周明杰
王荣
马文波
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention relates to a rare earth luminescent material, which comprises rare earth-aluminate (gallate) acid salt coated with metal nanometer particles, the composition general formula is Y3-xLnx(Al1-y Gay)5O12@M, wherein: 0<x<=0.5; Ln is at least one of cerium (Ce) and terbium (Tb); 0<=y<1.0; @ expresses coating; M is at least one of metal nano particles of gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu); the mol ratio of M to Al is z, 0<z<=1*10<-2>. The rare earth luminescent material has the advantages of high luminescent efficiency. The invention also provides a method for preparing a rare earth luminescent material.

Description

Rare earth luminescent material and preparation method thereof
[technical field]
The present invention relates to a kind of luminescent material, relate in particular to a kind of luminescent material that contains rare earth element and preparation method thereof.
[background technology]
At present, rare earth luminescent material has developed into the important luminescent materials in field such as information demonstration, lighting source, photoelectric device as a kind of new and effective luminescent material.Can effectively improve the performance of luminescent device by the luminous intensity that improves rare earth luminescent material, improve the luminous efficiency of device and effectively energy-conservation simultaneously.Therefore, the research of the luminescent material of high-luminous-efficiency and application are the important research contents in materials chemistry and materials physics field always.
The fluorescent material of traditional use rare earth luminescent material preparation, for example Y 3(Al, Ga) 5O 12, having luminous intensity height, stable becoming better, advantages such as epigranular are mainly used in products such as color field emissive display, projection TV.Yet the luminous efficiency of above-mentioned fluorescent material remains further to be improved.
[summary of the invention]
Based on this, be necessary to provide higher rare earth luminescent material of a kind of luminous efficiency and preparation method thereof.
A kind of rare earth luminescent material comprises rare earth-aluminium (gallium) hydrochlorate that is coated with metal nanoparticle, and it forms general formula is Y 3-xLn x(Al 1-yGa y) 5O 12M, wherein: 0＜x≤0.5; Ln is cerium (Ce), at least a in the terbium (Tb); 0≤y＜1.0; Expression coats; M is at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle; The mol ratio of M and Al is z, 0＜z≤1 * 10 -2
Wherein, 0.01≤x≤0.3.
Wherein, 0.2≤y≤0.6.
Wherein, 1 * 10 -5≤ z≤5 * 10 -3
A kind of preparation method of above-mentioned rare earth luminescent material, comprise the steps: metal nanoparticle is joined in the solution of polyvinylpyrrolidone, stir, wherein metal nanoparticle is at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle; Add and contain Al 3+Solution and tensio-active agent, stir; Under 0～100 ℃, add precipitation agent, ageing behind stirring 1.5～5h, with sedimentation and filtration, washing, drying, wherein precipitation agent is NH 4HCO 3, NH 3H 2O, (NH 4) 2CO 3, at least a in the urea; Calcine the Al that 1～8h obtains being coated with metal nanoparticle down with being deposited in 500～1200 ℃ 2O 3Powder; According to Y 3-xLn x(Al 1-yGa y) 5O 12The ratio of M takes by weighing the compound of Y, Ga and Ln correspondence and is coated with the Al of metal nanoparticle 2O 3, ground and mixed is even; In the reaction 2～8 hours down of 1300～1700 ℃, reducing atmosphere, be cooled to room temperature, products therefrom is ground be powder.
Wherein, contain Al 3+Solution be AlCl 3Solution, Al 2(SO 4) 3Solution, Al (NO 3) 3At least a in the solution.
Wherein, tensio-active agent is at least a in polyoxyethylene glycol, ethylene glycol, Virahol, the polyvinyl alcohol.
Wherein, tensio-active agent is that molecular weight is the polyoxyethylene glycol of 2000-10000.
Wherein, reducing atmosphere is N 2With H 2Mix reducing atmosphere, carbon reducing agent atmosphere, CO reducing atmosphere, pure H 2At least a in the reducing atmosphere.
Wherein, the compound of Y, Ga and Ln correspondence is at least a in the oxide compound, muriate, carbonate, nitrate, oxalate of Y, Ga and Ln correspondence.
Above-mentioned rare earth luminescent material has produced surface phasmon (surface plasmon, SP) effect is to have reached the effect that strengthens luminous efficiency owing to be coated on metal ion outside rare earth-aluminium (gallium) hydrochlorate.The performance test results shows that above-mentioned rare earth luminescent material has higher light emission intensity at the range of wavelengths that draws 0-580nm.In addition, above-mentioned preparation method's technology is simple, equipment requirements is low, pollution-free, be easy to control, be suitable for suitability for industrialized production.
[description of drawings]
Fig. 1 is the Y of the embodiment of the invention 1 preparation 2.99Ce 0.01Al 5O 12The Pt luminescent material is luminescent spectrum figure under the cathode-ray exciting under the 3KV at acceleration voltage, is the peak of a broad, and strength is positioned at 540nm.
Fig. 2 is the Y of the embodiment of the invention 3 preparations 2.5Tb 0.50(Al 1-0.2Ga 0.2) 5O 12The Au luminescent material is luminescent spectrum figure under the cathode-ray exciting under the 5KV at acceleration voltage, and emission peak is positioned at the spike of 544nm.
[embodiment]
Below in conjunction with drawings and the embodiments rare earth luminescent material and preparation method thereof is described in detail.
The rare earth luminescent material that present embodiment provided is a kind of fluorescent material, and it is rare earth-aluminium (gallium) hydrochlorate that is coated with metal nanoparticle.The composition general formula of this rare earth luminescent material is Y 3-xLn x(Al 1-yGa y) 5O 12M, wherein: 0＜x≤0.5 is preferably 0.01≤x≤0.3; Ln is cerium (Ce), at least a in the terbium (Tb); 0≤y＜1.0 are preferably 0.2≤y≤0.6; Expression coats; M is at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle; The mol ratio of M and Al is z, 0＜z≤1 * 10 -2, be preferably 1 * 10 -5≤ z≤5 * 10 -3
The preparation method of above-mentioned rare earth luminescent material comprises the steps:
(1) metal nanoparticle is carried out surface treatment, to stir in the solution that at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle join polyvinylpyrrolidone.
(2) add in the above-mentioned solution and contain Al 3+Solution and tensio-active agent, stir.Wherein, this contains Al 3+Solution be preferably AlCl 3Solution, Al 2(SO 4) 3Solution, Al (NO 3) 3At least a in the solution.This tensio-active agent is at least a in polyoxyethylene glycol, ethylene glycol, Virahol, the polyvinyl alcohol, is preferably the polyoxyethylene glycol that molecular weight is 2000-10000.
(3) slowly drip precipitation agent under 0～100 ℃ water bath condition, ageing behind stirring 1.5～5h is then with sedimentation and filtration, washing, drying.Wherein, precipitation agent is NH 4HCO 3, NH 3H 2O, (NH 4) 2CO 3, at least a in the urea.
(4) will be deposited in 500～1200 ℃ of calcining 1～8h down, to obtain being coated with the Al of metal nanoparticle 2O 3Powder.
(5) according to Y 3-xLn x(Al 1-yGa y) 5O 12The ratio of M takes by weighing compound and this Al that is coated with metal nanoparticle of Y, Ga and Ln correspondence 2O 3, ground and mixed is even.Wherein, the compound of Y, Ga and Ln correspondence is preferably at least a in the oxide compound, muriate, carbonate, nitrate, oxalate of Y, Ga and Ln correspondence.
(6) calcination 2～8 hours under 1300～1700 ℃, reducing atmosphere is cooled to room temperature, products therefrom is ground be powder.Wherein reducing atmosphere is preferably N 2With H 2Mix reducing atmosphere, carbon reducing agent atmosphere, CO reducing atmosphere, pure H 2At least a in the reducing atmosphere.
Above-mentioned preparation method's technology is simple, equipment requirements is low, pollution-free, be easy to control, be suitable for suitability for industrialized production.
Preparation method to above-mentioned rare earth luminescent material is described further below by various embodiments.Following all reagent are analytical pure.
Embodiment 1
Under the room temperature, the polyvinylpyrrolidone (PVP) that takes by weighing 0.30g is dissolved in the 5mL deionized water, and dissolving adds 6mL 1 * 10 then -2The mol/L nano platinum particle stirs 18h, while then stir the AlCl that adds 12mL 1mol/L successively 3, Virahol 5mL, the back that stirs slowly drips 30mL 4mol/LNH 4HCO 3, stirring reaction 5 hours, ageing certain hour then.With sedimentation and filtration, washing, drying, obtain Al behind 500 ℃ of thermal treatment 8h 2O 3The powder of Pt, wherein Al: Pt=1: 5 * 10 -3Take by weighing the Y of 1.0698g then 2(CO 3) 3, the Al of 0.5098g 2O 3Pt, the Ce of 0.0046g 2(CO 3) 3, place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, in tube furnace at 95%N 2Add 5%H 2The following 1700 ℃ of calcination 2h of weakly reducing atmosphere are cooled to room temperature, grind to be can obtain Y by powder 2.99Ce 0.01Al 5O 12The Pt luminescent material.
Be illustrated in figure 1 as Y 2.99Ce 0.01Al 5O 12The Pt luminescent material is luminescent spectrum figure under the cathode-ray exciting under the 3KV at acceleration voltage, and emission peak is positioned at 540nm.Be a broad peak, jaundice light.
Embodiment 2
Under the room temperature, take by weighing 0.1g PVP and be dissolved in the 4mL deionized water, dissolving adds 6mL1 * 10 then -3Mol/L Ag nanoparticle stirs 12h, while then stir the Al (NO that adds 6mL 2mol/L successively 3) 3, the polyvinyl alcohol water solution 6mL of 4% (V/V) slowly drips NH under the back vigorous stirring that stirs 3H 2O, until pH=9, stirring reaction 3 hours, ageing certain hour then.With sedimentation and filtration, washing, drying, obtain Al behind 900 ℃ of thermal treatment 4h 2O 3The powder of Ag, wherein Al: Ag=1: 2.5 * 10 -4Take by weighing the Y of 0.6322g then 2O 3, the Al of 0.5098g 2O 3Ag, the CeO of 0.0275g 2, the Tb of 0.0448g 4O 7Place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, in retort furnace, adopt carbon reducing agent, 1500 ℃ of calcination 4h are cooled to room temperature, grind to be can obtain Y by powder 2.80Tb 0.12Ce 0.08Al 5O 12The Ag luminescent material.
Embodiment 3
Under the room temperature, take by weighing 0.15g PVP and be dissolved in the 4mL deionized water, dissolving adds 10mL1 * 10 then -2Mol/L Au nanoparticle stirs 12h, while then stir the Al (NO that adds 10mL 1mol/L successively 3) 3, the molecular weight of 5% (V/V) is 2000 polyoxyethylene glycol (PEG2000) aqueous solution 10mL, slowly drips 20mL 2mol/L (NH then 4) 2CO 3, stirring reaction 4 hours, ageing certain hour then.With sedimentation and filtration, washing, drying, obtain Al behind 1000 ℃ of thermal treatment 1.5h 2O 3The powder of Au, wherein Al: Au=1: 1 * 10 -2Take by weighing the Y of 0.5645g then 2O 3, the Al of 0.4078g 2O 3Au, the Ga of 0.1874g 2O 3, the Tb of 0.1868g 4O 7, place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, in tube furnace at 95%N 2Add the following 1450 ℃ of calcination 6h of 5%H2 weakly reducing atmosphere, be cooled to room temperature, grind and be to obtain Y by powder 2.5Tb 0.50(Al 1-0.2Ga 0.2) 5O 12The Au luminescent material.
Be illustrated in figure 2 as Y 2.5Tb 0.50(Al 1-0.2Ga 0.2) 5O 12The Au luminescent material is luminescent spectrum figure under the cathode-ray exciting under the 5KV at acceleration voltage, and emission is positioned at the green glow at 544nm place.
Embodiment 4
Under the room temperature, take by weighing 0.20g PVP and be dissolved in the 5mL deionized water, dissolving adds 5mL 8 * 10 then -3Mol/L Pd nanoparticle stirs 12h, while then stir the Al that adds 5mL 1mol/L successively 2(SO 4) 3, the PEG100 aqueous solution 10mL of 10% (V/V) slowly drips 20mL 2mol/L urea then, and stirring reaction is 2.5 hours under 100 ℃ of water-baths, then the ageing certain hour.With sedimentation and filtration, washing, drying, obtain Al behind 1200 ℃ of thermal treatment 1h 2O 3The powder of Pd, wherein Al: Pd=1: 4 * 10 -3Take by weighing the Y (NO of 1.4844g then 3) 3, the Al of 0.2039g 2O 3Pd, the Ga (NO of 1.5344g 3) 3, the Ce (NO of 0.0652g 3) 3, the Tb (NO of 0.1379g 3) 3Place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, 1400 ℃ of thermal treatment 6h in retort furnace, again in tube furnace at 95%N 2Add 5%H 2The following 1400 ℃ of calcination 4h of weakly reducing atmosphere are cooled to room temperature, grind to be can obtain Y by powder 2.7Ce 0.10Tb 0.20(Al 0.4Ga 0.6) 5O 12The Pd luminescent material.
Embodiment 5
Under the room temperature, take by weighing 0.08g PVP and be dissolved in the 8mL deionized water, dissolving adds 1mL 1 * 10 then -4Mol/L Ag nanoparticle stirs 18h, while then stir the Al (NO that adds 5mL 2mol/L successively 3) 3, ethylene glycol 3mL slowly drips NH then 3H 2O, until pH=9, then stirring reaction is 2 hours, then the ageing certain hour.With sedimentation and filtration, washing, drying, obtain Al behind 800 ℃ of thermal treatment 4h 2O 3The powder of Ag, wherein Al: Ag=1: 1 * 10 -5Take by weighing the Y of 1.2723g then 2(C 2O 4) 3, the Al of 0.3568g 2O 3Ag, the Ga of 0.6051g 2(C 2O 4) 3, the Ce of 0.0653g 2(C 2O 4) 3, place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, 1300 ℃ of calcination 8h reduction under the CO reducing atmosphere is cooled to room temperature in tube furnace, grinds to be can obtain Y by powder 2.88Ce 0.12(Al 0.7Ga 0.3) 5O 12The Ag luminescent material.
Embodiment 6
Under the room temperature, take by weighing 0.18g PVP and be dissolved in the 8mL deionized water, dissolving adds 2mL 3 * 10 then -3Mol/L Cu nanoparticle stirs 24h, while then stir the AlCl that adds 12mL 1mol/L successively 3, the PEG10000 aqueous solution 8mL of 5% (V/V), the back that stirs slowly drips 30mL 3mol/LNH 4HCO 3, stirring reaction is 5 hours under 60 ℃ of water-baths, ageing certain hour then, and filtration, washing, drying obtain Al behind 600 ℃ of thermal treatment 6h 2O 3The powder of Cu, wherein Al: Cu=1: 5 * 10 -4Take by weighing the YCl of 1.0544g then 3, the Al of 0.5098g 2O 3Cu, the TbCl of 0.1591g 3, place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, 1600 ℃ of thermal treatment 3h in retort furnace, again in tube furnace at 95%N 2Add 5%H 2The following 1400 ℃ of calcination 2h of weakly reducing atmosphere, be cooled to room temperature, grind and be can obtain Y by powder 2.70Tb 0.30Al 5O 12The Cu luminescent material.
Embodiment 7
Under the room temperature, take by weighing 0.5g PVP and be dissolved in the 10mL deionized water, dissolving adds 4mL 3 * 10 then -4Mol/L Au metal nanoparticle stirs 24h, while then stir the Al that adds 6mL 1mol/L successively 2(SO 4) 3, the PEG20000 aqueous solution 5mL of 5% (V/V) slowly drips 20mL 3mol/L urea then, and stirring reaction is 1.5 hours under 80 ℃ of water-baths, then the ageing certain hour.With sedimentation and filtration, washing, drying, obtain Al behind 800 ℃ of thermal treatment 2h 2O 3The powder of Au, wherein Al: Au=1: 2 * 10 -4Take by weighing the Y of 1.0018g then 2(CO 3) 3, the Al of 0.4588g 2O 3Au, the Ce of 0.0690g 2(CO 3) 3, the Tb of 0.0248g 2(CO 3) 3Place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, in tube furnace at H 2The following 1500 ℃ of calcination 3h of reducing atmosphere are cooled to room temperature, grind to be can obtain Y by powder 2.80Ce 0.15Tb 0.05(Al 0.9Ga 0.1) 5O 12The Au luminescent material.
Embodiment 8
Under the room temperature, take by weighing 0.25g PVP and be dissolved in the 6mL deionized water, dissolving adds 3mL 1 * 10 then -3Mol/L Pt metal nanoparticle stirs 24h, while then stir the AlCl that adds 15mL 1mol/L successively 3, ethylene glycol 5mL, the back that stirs slowly drips 20mL 5mol/L (NH 4) 2CO 3, stirring reaction is 3 hours under 70 ℃ of water-baths, ageing certain hour then, and filtration, washing, drying obtain Al behind 900 ℃ of thermal treatment 3h 2O 3The powder of Pt, wherein Al: Pt=1: 2 * 10 -4Take by weighing the Y (NO of 1.5944g then 3) 3, the Al of 0.5098g 2O 3Pt, the Ce (NO of 0.0652g 3) 3, place agate mortar fully to be ground to and mix, then with powder transfer in corundum crucible, 1400 ℃ of calcination 5h under the common reducing atmosphere of building of carbon dust and CO are cooled to room temperature, grind to be can obtain Y by powder 2.90Ce 0.10Al 5O 12The Pt luminescent material.
In addition, those skilled in the art can also do other variation in spirit of the present invention, and certainly, these are included within the scope of protection of present invention according to the variation that spirit of the present invention is done.

Claims (10)

1. a rare earth luminescent material is characterized in that, comprises rare earth-aluminium (gallium) hydrochlorate that is coated with metal nanoparticle, and it forms general formula is Y 3-xLn x(Al 1-yGa y) 5O 12M, wherein:
0＜x≤0.5；
Ln is cerium (Ce), at least a in the terbium (Tb);
0≤y＜1.0；
Expression coats;
M is at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle;
The mol ratio of M and Al is z, 0＜z≤1 * 10 -2
2. rare earth luminescent material as claimed in claim 1 is characterized in that: 0.01≤x≤0.3.
3. rare earth luminescent material as claimed in claim 1 is characterized in that: 0.2≤y≤0.6.
4. rare earth luminescent material as claimed in claim 1 is characterized in that: 1 * 10 -5≤ z≤5 * 10 -3
5. the preparation method of a rare earth luminescent material as claimed in claim 1 comprises the steps:
Metal nanoparticle is joined in the solution of polyvinylpyrrolidone, stir; Wherein, this metal nanoparticle is at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle;
Add and contain Al 3+Solution and tensio-active agent, stir;
Add precipitation agent under 0～100 ℃, ageing behind stirring 1.5～5h is with sedimentation and filtration, washing, drying; Wherein, this precipitation agent is NH 4HCO 3, NH 3H 2O, (NH 4) 2CO 3, at least a in the urea;
Calcine the Al that 1～8h obtains being coated with metal nanoparticle down with being deposited in 500～1200 ℃ 2O 3Powder;
According to Y 3-xLn x(Al 1-yGa y) 5O 12The ratio of M takes by weighing compound and this Al that is coated with metal nanoparticle of Y, Ga and Ln correspondence 2O 3, ground and mixed is even;
In the reaction 2～8 hours down of 1300～1700 ℃, reducing atmosphere, be cooled to room temperature, products therefrom is ground be powder.
6. the preparation method of rare earth luminescent material as claimed in claim 5, it is characterized in that: this contains Al 3+Solution be AlCl 3Solution, Al 2(SO 4) 3Solution, Al (NO 3) 3At least a in the solution.
7. the preparation method of rare earth luminescent material as claimed in claim 5 is characterized in that: this tensio-active agent is at least a in polyoxyethylene glycol, ethylene glycol, Virahol, the polyvinyl alcohol.
8. the preparation method of rare earth luminescent material as claimed in claim 7, it is characterized in that: this tensio-active agent is that molecular weight is the polyoxyethylene glycol of 2000-10000.
9. the preparation method of rare earth luminescent material as claimed in claim 5, it is characterized in that: this reducing atmosphere is N 2With H 2Mix reducing atmosphere, carbon reducing agent atmosphere, CO reducing atmosphere, pure H 2At least a in the reducing atmosphere.
10. the preparation method of rare earth luminescent material as claimed in claim 5 is characterized in that: the compound of this Y, Ga and Ln correspondence is at least a in the oxide compound of Y, Ga and Ln correspondence, muriate, carbonate, nitrate, the oxalate.
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WO2014067109A1 (en) * 2012-10-31 2014-05-08 海洋王照明科技股份有限公司 Aluminate luminescent material and preparation method therefor
CN103881715A (en) * 2012-12-20 2014-06-25 海洋王照明科技股份有限公司 Calcium silicate red light emitting material and preparation method thereof
CN104119910A (en) * 2013-04-28 2014-10-29 广东超越光电科技有限公司 Fluorescent powder for light-emitting diode
CN104204133A (en) * 2012-07-31 2014-12-10 海洋王照明科技股份有限公司 Zinc aluminate material and method for preparing same

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CN102812107A (en) * 2010-05-25 2012-12-05 海洋王照明科技股份有限公司 Aluminate-based Fluorescent Powder Coated By Metal Nanoparticle And Production Method Thereof

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JP2005008844A (en) * 2003-02-26 2005-01-13 Nichia Chem Ind Ltd Phosphor, and light emitter using the same
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CN104204133A (en) * 2012-07-31 2014-12-10 海洋王照明科技股份有限公司 Zinc aluminate material and method for preparing same
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CN103881715A (en) * 2012-12-20 2014-06-25 海洋王照明科技股份有限公司 Calcium silicate red light emitting material and preparation method thereof
CN104119910A (en) * 2013-04-28 2014-10-29 广东超越光电科技有限公司 Fluorescent powder for light-emitting diode

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