CN102277172B - Rare earth luminescent material and its preparation method - Google Patents
Rare earth luminescent material and its preparation method Download PDFInfo
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- CN102277172B CN102277172B CN2010102022609A CN201010202260A CN102277172B CN 102277172 B CN102277172 B CN 102277172B CN 2010102022609 A CN2010102022609 A CN 2010102022609A CN 201010202260 A CN201010202260 A CN 201010202260A CN 102277172 B CN102277172 B CN 102277172B
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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
[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, as a kind of new and effective luminescent material, has developed into the important luminescent materials in field such as information demonstration, lighting source, photoelectric device.By the luminous intensity that improves rare earth luminescent material, can effectively improve the performance of luminescent device, the luminous efficiency that improves simultaneously device is also effectively energy-conservation.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.
Fluorescent material prepared by traditional use rare earth luminescent material, for example Y
3(Al, Ga)
5O
12, having that luminous intensity is high, stable becomes better, the advantages such as epigranular, be mainly used in the 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 rare earth luminescent material that a kind of luminous efficiency is higher and preparation method thereof.
A kind of rare earth luminescent material, comprise 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
12@M, wherein: 0<x≤0.5; Ln is cerium (Ce), at least a in terbium (Tb); 0≤y<1.0; @means to coat; 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 after stirring 1.5～5h, by sedimentation and filtration, washing, drying, wherein precipitation agent is NH
4HCO
3, NH
3H
2O, (NH
4)
2CO
3, at least a in urea; By being deposited under 500～1200 ℃, calcine the Al that 1～8h obtains being coated with metal nanoparticle
2O
3Powder; According to Y
3-xLn
x(Al
1-yGa
y)
5O
12The ratio of@M, take the compound that Y, Ga and Ln are corresponding and be coated with the Al of metal nanoparticle
2O
3, ground and mixed is even; Under 1300～1700 ℃, reducing atmosphere, reacted 2～8 hours, be cooled to room temperature, products therefrom is ground to powder.
Wherein, contain Al
3+Solution be AlCl
3Solution, Al
2(SO
4)
3Solution, Al (NO
3)
3At least a in solution.
Wherein, tensio-active agent is at least a in polyoxyethylene glycol, ethylene glycol, Virahol, 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 reducing atmosphere.
Wherein, the compound that Y, Ga and Ln are corresponding is at least a in oxide compound that Y, Ga and Ln are corresponding, muriate, carbonate, nitrate, oxalate.
Above-mentioned rare earth luminescent material, because the metal ion be coated on outside rare earth-aluminium (gallium) hydrochlorate has produced surface phasmon (surface plasmon, SP) effect, to reach the effect that strengthens luminous efficiency.The performance test results shows, 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 technique is simple, equipment requirements is low, pollution-free, be easy to control, be suitable for suitability for industrialized production.
[accompanying drawing explanation]
Fig. 1 is the Y of the embodiment of the present invention 1 preparation
2.99Ce
0.01Al
5O
12@Pt luminescent material is the luminescent spectrum figure under the cathode-ray exciting under 3KV at acceleration voltage, is that a wider ，Zui strength, peak is positioned at 540nm.
Fig. 2 is the Y of the embodiment of the present invention 3 preparations
2.5Tb
0.50(Al
1-0.2Ga
0.2)
5O
12@Au luminescent material is the luminescent spectrum figure under the cathode-ray exciting under 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 provides 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
12@M, wherein: 0<x≤0.5 is preferably 0.01≤x≤0.3; Ln is cerium (Ce), at least a in terbium (Tb); 0≤y<1.0, be preferably 0.2≤y≤0.6; @means to coat; 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 to surface treatment,, in solution that at least a in gold (Au), silver (Ag), platinum (Pt), palladium (Pd) and copper (Cu) metal nanoparticle join polyvinylpyrrolidone, to stir.
(2) toward adding in above-mentioned solution, 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 solution.This tensio-active agent is at least a in polyoxyethylene glycol, ethylene glycol, Virahol, polyvinyl alcohol, is preferably the polyoxyethylene glycol that molecular weight is 2000-10000.
(3) under the water bath condition of 0～100 ℃, slowly drip precipitation agent, ageing after stirring 1.5～5h, then by sedimentation and filtration, washing, drying.Wherein, precipitation agent is NH
4HCO
3, NH
3H
2O, (NH
4)
2CO
3, at least a in urea.
(4) will be deposited under 500～1200 ℃ and calcine 1～8h, 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, take compound and this Al that is coated with metal nanoparticle that Y, Ga and Ln are corresponding
2O
3, ground and mixed is even.Wherein, the compound that Y, Ga and Ln are corresponding is preferably at least a in Y, Ga and oxide compound corresponding to Ln, muriate, carbonate, nitrate, oxalate.
(6) calcination 2～8 hours under 1300～1700 ℃, reducing atmosphere, be cooled to room temperature, and products therefrom is ground to 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 reducing atmosphere.
Above-mentioned preparation method's technique 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 is analytical pure.
Embodiment 1
Under room temperature, the polyvinylpyrrolidone (PVP) that takes 0.30g is dissolved in the 5mL deionized water, dissolves, and then adds 6mL 1 * 10
-2The mol/L nano platinum particle, stir 18h, while then stir the AlCl that adds successively 12mL 1mol/L
3, Virahol 5mL, rear slow dropping 30mL 4mol/LNH stirs
4HCO
3, stirring reaction 5 hours, then ageing certain hour.By sedimentation and filtration, washing, drying, obtain Al after 500 ℃ of thermal treatment 8h
2O
3The powder of@Pt, wherein Al: Pt=1: 5 * 10
-3.Then take the Y of 1.0698g
2(CO
3)
3, the Al of 0.5098g
2O
3@Pt, the Ce of 0.0046g
2(CO
3)
3, be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, in tube furnace at 95%N
2Add 5%H
2The lower 1700 ℃ of calcination 2h of weakly reducing atmosphere, be cooled to room temperature, is ground to powder, can obtain Y
2.99Ce
0.01Al
5O
12@Pt luminescent material.
Be illustrated in figure 1 Y
2.99Ce
0.01Al
5O
12@Pt luminescent material is the luminescent spectrum figure under the cathode-ray exciting under 3KV at acceleration voltage, and emission peak is positioned at 540nm.Be a broad peak, Yellow light-emitting low temperature.
Embodiment 2
Under room temperature, take 0.1g PVP and be dissolved in the 4mL deionized water, dissolve, then add 6mL1 * 10
-3Mol/L Ag nanoparticle, stir 12h, while then stir the Al (NO that adds successively 6mL 2mol/L
3)
3, the polyvinyl alcohol water solution 6mL of 4% (V/V), slowly drip NH under the rear vigorous stirring that stirs
3H
2O, until pH=9, stirring reaction 3 hours, then ageing certain hour.By sedimentation and filtration, washing, drying, obtain Al after 900 ℃ of thermal treatment 4h
2O
3The powder of@Ag, wherein Al: Ag=1: 2.5 * 10
-4.Then take the Y of 0.6322g
2O
3, the Al of 0.5098g
2O
3@Ag, the CeO of 0.0275g
2, the Tb of 0.0448g
4O
7Be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, in retort furnace, adopt carbon reducing agent, 1500 ℃ of calcination 4h, be cooled to room temperature, is ground to powder, can obtain Y
2.80Tb
0.12Ce
0.08Al
5O
12@Ag luminescent material.
Embodiment 3
Under room temperature, take 0.15g PVP and be dissolved in the 4mL deionized water, dissolve, then add 10mL1 * 10
-2Mol/L Au nanoparticle, stir 12h, while then stir the Al (NO that adds successively 10mL 1mol/L
3)
3, the molecular weight of 5% (V/V) is 2000 polyoxyethylene glycol (PEG2000) aqueous solution 10mL, then slowly drips 20mL 2mol/L (NH
4)
2CO
3, stirring reaction 4 hours, then ageing certain hour.By sedimentation and filtration, washing, drying, obtain Al after 1000 ℃ of thermal treatment 1.5h
2O
3The powder of@Au, wherein Al: Au=1: 1 * 10
-2.Then take the Y of 0.5645g
2O
3, the Al of 0.4078g
2O
3@Au, the Ga of 0.1874g
2O
3, the Tb of 0.1868g
4O
7, be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, in tube furnace at 95%N
2Add the lower 1450 ℃ of calcination 6h of 5%H2 weakly reducing atmosphere, be cooled to room temperature, be ground to powder, can obtain Y
2.5Tb
0.50(Al
1-0.2Ga
0.2)
5O
12@Au luminescent material.
Be illustrated in figure 2 Y
2.5Tb
0.50(Al
1-0.2Ga
0.2)
5O
12@Au luminescent material is the luminescent spectrum figure under the cathode-ray exciting under 5KV at acceleration voltage, and emission is positioned at the green glow at 544nm place.
Embodiment 4
Under room temperature, take 0.20g PVP and be dissolved in the 5mL deionized water, dissolve, then add 5mL 8 * 10
-3Mol/L Pd nanoparticle, stir 12h, while then stir the Al that adds successively 5mL 1mol/L
2(SO
4)
3, the PEG100 aqueous solution 10mL of 10% (V/V), then slowly drip 20mL 2mol/L urea, and under 100 ℃ of water-baths, stirring reaction is 2.5 hours, then the ageing certain hour.By sedimentation and filtration, washing, drying, obtain Al after 1200 ℃ of thermal treatment 1h
2O
3The powder of@Pd, wherein Al: Pd=1: 4 * 10
-3.Then take the Y (NO of 1.4844g
3)
3, the Al of 0.2039g
2O
3@Pd, the Ga (NO of 1.5344g
3)
3, the Ce (NO of 0.0652g
3)
3, the Tb (NO of 0.1379g
3)
3Be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, 1400 ℃ of thermal treatment 6h in retort furnace, then in tube furnace at 95%N
2Add 5%H
2The lower 1400 ℃ of calcination 4h of weakly reducing atmosphere, be cooled to room temperature, is ground to powder, can obtain Y
2.7Ce
0.10Tb
0.20(Al
0.4Ga
0.6)
5O
12@Pd luminescent material.
Embodiment 5
Under room temperature, take 0.08g PVP and be dissolved in the 8mL deionized water, dissolve, then add 1mL 1 * 10
-4Mol/L Ag nanoparticle, stir 18h, while then stir the Al (NO that adds successively 5mL 2mol/L
3)
3, ethylene glycol 3mL, then slowly drip NH
3H
2O, until pH=9, then stirring reaction is 2 hours, then the ageing certain hour.By sedimentation and filtration, washing, drying, obtain Al after 800 ℃ of thermal treatment 4h
2O
3The powder of@Ag, wherein Al: Ag=1: 1 * 10
-5.Then take the Y of 1.2723g
2(C
2O
4)
3, the Al of 0.3568g
2O
3@Ag, the Ga of 0.6051g
2(C
2O
4)
3, the Ce of 0.0653g
2(C
2O
4)
3, be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, 1300 ℃ of calcination 8h reduction under the CO reducing atmosphere, be cooled to room temperature in tube furnace, is ground to powder, can obtain Y
2.88Ce
0.12(Al
0.7Ga
0.3)
5O
12@Ag luminescent material.
Embodiment 6
Under room temperature, take 0.18g PVP and be dissolved in the 8mL deionized water, dissolve, then add 2mL 3 * 10
-3Mol/L Cu nanoparticle, stir 24h, while then stir the AlCl that adds successively 12mL 1mol/L
3, the PEG10000 aqueous solution 8mL of 5% (V/V), rear slow dropping 30mL 3mol/LNH stirs
4HCO
3, under 60 ℃ of water-baths, stirring reaction is 5 hours, ageing certain hour then, and filtration, washing, drying, obtain Al after 600 ℃ of thermal treatment 6h
2O
3The powder of@Cu, wherein Al: Cu=1: 5 * 10
-4.Then take the YCl of 1.0544g
3, the Al of 0.5098g
2O
3@Cu, the TbCl of 0.1591g
3, be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, 1600 ℃ of thermal treatment 3h in retort furnace, then in tube furnace at 95%N
2Add 5%H
2The lower 1400 ℃ of calcination 2h of weakly reducing atmosphere, be cooled to room temperature, be ground to powder, can obtain Y
2.70Tb
0.30Al
5O
12@Cu luminescent material.
Embodiment 7
Under room temperature, take 0.5g PVP and be dissolved in the 10mL deionized water, dissolve, then add 4mL 3 * 10
-4Mol/L Au metal nanoparticle, stir 24h, while then stir the Al that adds successively 6mL 1mol/L
2(SO
4)
3, the PEG20000 aqueous solution 5mL of 5% (V/V), then slowly drip 20mL 3mol/L urea, and under 80 ℃ of water-baths, stirring reaction is 1.5 hours, then the ageing certain hour.By sedimentation and filtration, washing, drying, obtain Al after 800 ℃ of thermal treatment 2h
2O
3The powder of@Au, wherein Al: Au=1: 2 * 10
-4.Then take the Y of 1.0018g
2(CO
3)
3, the Al of 0.4588g
2O
3@Au, the Ce of 0.0690g
2(CO
3)
3, the Tb of 0.0248g
2(CO
3)
3Be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, in tube furnace at H
2The lower 1500 ℃ of calcination 3h of reducing atmosphere, be cooled to room temperature, is ground to powder, can obtain Y
2.80Ce
0.15Tb
0.05(Al
0.9Ga
0.1)
5O
12@Au luminescent material.
Under room temperature, take 0.25g PVP and be dissolved in the 6mL deionized water, dissolve, then add 3mL 1 * 10
-3Mol/L Pt metal nanoparticle, stir 24h, while then stir the AlCl that adds successively 15mL 1mol/L
3, ethylene glycol 5mL, rear slow dropping 20mL 5mol/L (NH stirs
4)
2CO
3, under 70 ℃ of water-baths, stirring reaction is 3 hours, ageing certain hour then, and filtration, washing, drying, obtain Al after 900 ℃ of thermal treatment 3h
2O
3The powder of@Pt, wherein Al: Pt=1: 2 * 10
-4.Then take the Y (NO of 1.5944g
3)
3, the Al of 0.5098g
2O
3@Pt, the Ce (NO of 0.0652g
3)
3, be placed in agate mortar and fully be ground to and mix, then by powder transfer in corundum crucible, 1400 ℃ of calcination 5h under the common reducing atmosphere of building of carbon dust and CO, be cooled to room temperature, is ground to powder, can obtain Y
2.90Ce
0.10Al
5O
12@Pt luminescent material.
In addition, those skilled in the art can also do other variation in spirit of the present invention, and certainly, the variation that these are done according to spirit of the present invention, within being included in the scope of protection of present invention.
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
12@M, wherein:
0＜x≤0.5；
Ln is cerium (Ce);
0≤y＜1.0；
@means to coat;
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, comprise 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;
Under 0～100 ℃, add precipitation agent, ageing after stirring 1.5～5h, by sedimentation and filtration, washing, drying; Wherein, this precipitation agent is NH
4HCO
3, NH
3H
2O, (NH
4)
2CO
3, at least a in urea;
By being deposited under 500～1200 ℃, calcine the Al that 1～8h obtains being coated with metal nanoparticle
2O
3Powder;
According to Y
3-xLn
x(Al
1-yGa
y)
5O
12The ratio of@M, take compound and this Al that is coated with metal nanoparticle that Y, Ga and Ln are corresponding
2O
3, ground and mixed is even;
Under 1300～1700 ℃, reducing atmosphere, reacted 2～8 hours, be cooled to room temperature, products therefrom is ground to 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 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, 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 reducing atmosphere.
10. the preparation method of rare earth luminescent material as claimed in claim 5 is characterized in that: the compound that this Y, Ga and Ln are corresponding is at least a in oxide compound that Y, Ga and Ln are corresponding, muriate, carbonate, nitrate, oxalate.
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| WO2014019153A1 (en) * | 2012-07-31 | 2014-02-06 | 海洋王照明科技股份有限公司 | Zinc aluminate material and method for preparing same |
| JP6009091B2 (en) * | 2012-10-31 | 2016-10-19 | オーシャンズ キング ライティング サイエンスアンドテクノロジー カンパニー リミテッド | Aluminate luminescent material and method for producing the same |
| 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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|---|---|---|---|---|
| US6669866B1 (en) * | 1999-07-23 | 2003-12-30 | Patent-Treuhand-Gesellschaft Fuer Elektrische Gluehlampen Mbh | Luminous substance for a light source and light source associates therewith |
| CN1780896A (en) * | 2003-04-30 | 2006-05-31 | 纳米技术有限公司 | Luminescent core/shell nanoparticles |
| CN101181751A (en) * | 2007-12-17 | 2008-05-21 | 中国铝业股份有限公司 | Method for preparing nickel-coated alumina powder |
| 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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| JP4991026B2 (en) * | 2003-02-26 | 2012-08-01 | 日亜化学工業株式会社 | Light emitting device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6669866B1 (en) * | 1999-07-23 | 2003-12-30 | Patent-Treuhand-Gesellschaft Fuer Elektrische Gluehlampen Mbh | Luminous substance for a light source and light source associates therewith |
| CN1780896A (en) * | 2003-04-30 | 2006-05-31 | 纳米技术有限公司 | Luminescent core/shell nanoparticles |
| CN101181751A (en) * | 2007-12-17 | 2008-05-21 | 中国铝业股份有限公司 | Method for preparing nickel-coated alumina powder |
| 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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