CN103849383A - Manganese zinc aluminate luminescent material and preparation method thereof - Google Patents
Manganese zinc aluminate luminescent material and preparation method thereof Download PDFInfo
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- CN103849383A CN103849383A CN201210497265.8A CN201210497265A CN103849383A CN 103849383 A CN103849383 A CN 103849383A CN 201210497265 A CN201210497265 A CN 201210497265A CN 103849383 A CN103849383 A CN 103849383A
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Abstract
The invention belongs to the field of luminescent materials, and discloses a manganese zinc aluminate luminescent material and a preparation method thereof. The luminescent material has molecular formula of Zn1-xAl2O4:Mn<2+>x, My. M represents the doped metal nanoparticles and is at least one of Ag, Au, Pt, Pd and Cu metal nanoparticles, x is in the value range of: 0<x<=0.1, y represents the molar ratio of M and Al, and y is in the value range of: 0<y<=1*10<-2>. The manganese zinc aluminate luminescent material provided by the invention uses alumina aerogel to adsorb metal nanoparticles, in order to obtain the Al2O3 alumina aerogel containing metal nanoparticles; and then the Al2O3 alumina aerogel containing metal nanoparticles is used as a raw material to prepare the luminescent material. By doping metal nanoparticles, luminous intensity of the luminescent material is enhanced.
Description
Technical field
The present invention relates to luminescent material, relate in particular to a kind of aluminic acid zinc-manganese luminescent material and preparation method thereof.
Background technology
Field Emission Display (FED) is a kind of flat panel display that has very much development potentiality.The operating voltage of field emission display is lower than the operating voltage of cathode tube (CRT), be conventionally less than 5kV, and working current density is relatively large, generally at 10～100 μ Acm
-2.Therefore, higher to the requirement of the luminescent powder for Field Emission Display, as to have better saturation, luminous efficiency under low voltage higher and at close ℃ of high electric current without luminance saturation phenomenon etc.At present, the research of Field Emission Display luminescent powder is mainly concentrated on to two aspects: the one, utilize and improve existing cathode tube luminescent powder; The 2nd, find new luminescent material.Commercial cathodoluminescence powder, take sulfide as main, in the time being used for fabricating yard emission display screen, because sulphur wherein can react with Microamounts of Mo, silicon or germanium etc. in negative electrode, thereby having weakened its electron emission, and then has affected the performance of whole device.Exist potential using value in luminescent material Application Areas.
Aluminic acid zinc-manganese (ZnAl
2o
4) be a kind of semiconductor material with wide forbidden band with cubic spinel structure.ZnAl
2o
4the optical band gap of polycrystal powder is generally about 318～319eV, and chemical stability and thermostability are all very good, exist potential using value in luminescent material Application Areas.
Summary of the invention
Based on the problems referred to above, problem to be solved by this invention is to provide a kind of aluminic acid zinc-manganese luminescent material.
Technical scheme of the present invention is as follows:
A kind of aluminic acid zinc-manganese luminescent material, its general molecular formula is: Zn
1-xal
2o
4: Mn
2+ x, M
y; Wherein, M is metal nano particle-doped, and M is at least one in Ag, Au, Pt, Pd and Cu metal nanoparticle, and the span of x is 0 < x≤0.1, y is the mol ratio of M and Al, and the span of y is 0 < y≤1 × 10
-2.
Described aluminic acid zinc-manganese luminescent material, preferably, the span of x is 1 × 10
-3≤ x≤5 × 10
-2, the span of y is 1 × 10
-5≤ y≤5 × 10
-3.
Described aluminic acid zinc-manganese luminescent material, preferably, M is that mol ratio is Ag and the Au of 1: 1.
The present invention also provides a kind of preparation method of aluminic acid zinc-manganese luminescent material, comprises the steps:
S1, alumina aerogels is dissolved in the ethanolic soln of M salt, at 50～75 ℃, stir 0.5～3h, then ultrasonic 10min, dry at 60-150 ℃ again, by even dried former abrasive lapping, at 600～1200 ℃, calcine 0.5～4h, make the alumina aerogels that contains M nanoparticle; Wherein, the mol ratio of aluminum oxide and M is less than or equal to 5 × 10 for being greater than 0
-3;
S2, according to general molecular formula Zn
1-xal
2o
4: Mn
2+ x, M
yin the stoichiometric ratio of each element, take the alumina aerogels that includes M nanoparticle making in compound that Zn and Mn are corresponding and step S1, ground and mixed is even, be warming up to 800 ℃～1400 ℃ precalcinings 2～15 hours, in air atmosphere or reducing atmosphere, calcine 0.5～6 hour in 1000 ℃～1400 ℃ again, furnace cooling is cooled to room temperature, and obtained sample is ground to powder, and obtaining general molecular formula is Zn
1-xal
2o
4: Mn
2+ x, M
yaluminic acid zinc-manganese luminescent material;
In above-mentioned steps, M is metal nano particle-doped, and M is at least one in Ag, Au, Pt, Pd and Cu metal nanoparticle, and the span of x is 0 < x≤0.1, y is the mol ratio of M and Al, and the span of y is 0 < y≤1 × 10
-2.
The preparation method of described aluminic acid zinc-manganese luminescent material, in step S1, the concentration of the ethanolic soln of M salt is 5 × 10
-6mol/L～1 × 10
-2mol/L.
The preparation method of described aluminic acid zinc-manganese luminescent material, in step S2, at least one in the nitrate of the oxide compound that the compound of Zn is Zn, the carbonate of Zn, Zn, the acetate of Zn and the oxalate of Zn.
The preparation method of described aluminic acid zinc-manganese luminescent material, in step S2, at least one in the nitrate of the oxide compound that the compound of Mn is Mn, the carbonate of Mn, Mn, the acetate of Mn and the oxalate of Mn.
Aluminic acid zinc-manganese luminescent material provided by the invention, this luminescent material adopts alumina aerogels adsorbing metal nanoparticle, obtains including the Al of metal nanoparticle
2o
3alumina aerogels, and then prepare as raw material take the alumina aerogels that includes metallics, like this by metal nano particle-doped, strengthen the luminous intensity of luminescent material; In addition, this material is due to doped with metal nanoparticle, and its chemical property and thermal characteristics are all highly stable.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of aluminic acid zinc-manganese luminescent material of the present invention;
Fig. 2 is that aluminic acid zinc-manganese luminescent material prepared by embodiment 3 is the luminescent spectrum comparison diagram under the cathode-ray exciting under 3KV with contrast luminescent material at acceleration voltage; Wherein, curve 1 is the aluminic acid zinc-manganese luminescent material that embodiment 3 makes: the Zn of metal nano particle-doped Ag
0.98al
2o
4: Mn
0.02,
the luminescent spectrum of aluminic acid zinc-manganese luminescent material; Curve 2 is contrast luminescent materials: not metal nano particle-doped Zn
0.98al
2o
4: Mn
0.02the luminescent spectrum of luminescent material.
Embodiment
Aluminic acid zinc-manganese luminescent material provided by the invention, its general molecular formula is: Zn
1-xal
2o
4: Mn
2+ x, M
y; Wherein, M is metal nano particle-doped, M is at least one in Ag, Au, Pt, Pd and Cu metal nanoparticle, the span of x is 0 < x≤0.1, y be metal nanoparticle M with luminescent material in Al mole ratio, the span of y is 0 < y≤1 × 10
-2; Preferably, the span of x is 1 × 10
-3≤ x≤5 × 10
-2, the span of y is 1 × 10
-5≤ y≤5 × 10
-3.
Preferably, M is that mol ratio is Ag and the Au of 1: 1.
Aluminic acid zinc-manganese luminescent material provided by the invention, this luminescent material adopts alumina aerogels adsorbing metal nanoparticle, obtains including the Al of metal nanoparticle
2o
3alumina aerogels, and then prepare as raw material take the alumina aerogels that includes metallics, like this by metal nano particle-doped, strengthen the luminous intensity of luminescent material; In addition, this material is due to doped with metal nanoparticle, and its chemical property and thermal characteristics are all highly stable.
The preparation method of above-mentioned aluminic acid zinc-manganese luminescent material, it comprises the steps:
S1: alumina aerogels is dissolved in the ethanolic soln of M salt, at 50～75 ℃, stir 0.5～3h, then ultrasonic 10min, dry at 60-150 ℃ again, by even dried former abrasive lapping, at 600～1200 ℃, calcine 0.5～4h, make the alumina aerogels that contains M nanoparticle; Wherein, the mol ratio of aluminum oxide and M is less than or equal to 5 × 10 for being greater than 0
-3, preferably, the mol ratio of aluminum oxide and M is 5 × 10
-6～2.5 × 10
-3
S2, according to general molecular formula Zn
1-xal
2o
4: Mn
2+ x, M
yin the stoichiometric ratio of each element, take the alumina aerogels that includes M nanoparticle making in compound that Zn and Mn are corresponding and step S1, ground and mixed is even, be warming up to 800 ℃～1400 ℃ precalcinings 2～15 hours, in air atmosphere or reducing atmosphere, calcine 0.5～6 hour in 1000 ℃～1400 ℃ again, furnace cooling is cooled to room temperature, and obtained sample is ground to powder, and obtaining general molecular formula is Zn
1-xal
2o
4: Mn
2+ x, M
yaluminic acid zinc-manganese luminescent material;
In above-mentioned steps, M is metal nano particle-doped, and M is at least one in Ag, Au, Pt, Pd and Cu metal nanoparticle, and the span of x is 0 < x≤0.1, y is the mol ratio of M and Al, and the span of y is 0 < y≤1 × 10
-2.
The preparation method of described aluminic acid zinc-manganese luminescent material, in step S1, the compound of described Zn and Mn is oxide compound, carbonate, nitrate, acetate or the oxalate of Zn and Mn; That is: at least one in nitrate, the acetate of Zn and the oxalate of Zn of the oxide compound that the compound of Zn is Zn, the carbonate of Zn, Zn; The compound of Mn is at least one in nitrate, the acetate of Mn and the oxalate of Mn of carbonate, Mn of oxide compound, the Mn of Mn.
The preparation method of described aluminic acid zinc-manganese luminescent material, in step S2, described reducing atmosphere is that volume ratio is the N of 95: 5
2with H
2reducing atmosphere, carbon reducing agent atmosphere, the pure H of composition
2at least one in reducing atmosphere.
In the preparation method of described aluminic acid zinc-manganese luminescent material, preferably, the span of x is 1 × 10
-3≤ x≤5 × 10
-2, the span of y is 1 × 10
-5≤ y≤5 × 10
-3; Preferably, M is that mol ratio is Ag and the Au of 1: 1.
In above-mentioned aluminic acid zinc-manganese luminescent material and preparation method thereof, strengthened its luminous intensity by metal nano particle-doped, and prepared aluminic acid zinc-manganese luminescent material has good stability, the advantage of good luminous performance; Preparation method's technique of the present invention is simple, equipment requirements is low, pollution-free, be easy to control, be suitable for suitability for industrialized production, there is wide production application prospect.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1:Zn
0.999al
2o
4: Mn
2+ 0.001,
First take alumina aerogels 0.6116g, be dissolved into 24ml and contain Palladous chloride (PdCl
22H
2o) 5 × 10
-6in the ethanolic soln of mol/L, at 65 ℃, stir 1.5h, then ultrasonic 10min, then be dried at 120 ℃, dried sample is ground evenly, precalcining 2h at 1100 ℃, obtains the alumina aerogels that contains metal ion.
Then take ZnC
2o
42H
2o 0.7569g, the Al that contains metal ion of 0.4078g
2o
3aerogel, MnC
2o
42H
2o 0.0006g, is placed in agate mortar and is fully ground to and mixes, then by powder transfer in corundum crucible, in retort furnace at 1400 ℃ of thermal treatment 2h, in the lower 1400 ℃ of sintering 0.5h of weak reducing atmosphere of CO, be cooled to room temperature again, can obtain the Zn of doping Pd
0.999al
2o
4: Mn
2+ 0.001,
luminescent material.
Embodiment 2:Zn
0.98al
2o
4: Mn
0.01,
First take alumina aerogels 0.6117g, be dissolved into 12ml and contain hydrochloro-auric acid (HAuCl
4) 1 × 10
-2in the ethanolic soln of mol/L, at 75 ℃, stir 0.5h, then ultrasonic 10min, then be dried at 150 ℃, dried sample is ground evenly, precalcining 0.5h at 1200 ℃, obtains the alumina aerogels that contains metal ion.
Then take ZnCO
30.3073g, the Al that contains metal ion
2o
3aerogel 0.2549g, MnCO
30.0028g, is placed in agate mortar and is fully ground to and mixes, then by powder transfer in corundum crucible, 800 ℃ of thermal treatment 15h in retort furnace, then under 1000 ℃ of air atmospheres sintering 4h, be cooled to room temperature, can obtain the Zn of doping metals
0.98al
2o
4: Mn
0.01,
luminescent material.
Embodiment 3:Zn
0.98al
2o
4: Mn
0.02,
First take alumina aerogels 0.3058g, be dissolved into 7.5ml and contain Silver Nitrate (AgNO
3) 2 × 10
-4in the ethanolic soln of mol/L, at 60 ℃, stir 2h, then ultrasonic 10min, then be dried at 80 ℃, dried sample is ground evenly, precalcining 2h at 800 ℃, obtains the alumina aerogels that contains metal ion.
Then take ZnO 0.3223g, the Al that contains metal ion
2o
3aerogel 0.4078g, MnO
20.0069g, is placed in agate mortar and is fully ground to and mixes, then by powder transfer in corundum crucible, 1250 ℃ of thermal treatment 4h in retort furnace, then the N that is 95: 5 in volume ratio in tube furnace
2with H
2the lower 1200 ℃ of sintering 2h reduction of weakly reducing atmosphere of composition, is cooled to room temperature, can obtain the Zn of doping metals Ag
0.98al
2o
4: Mn
0.02,
luminescent material.
Fig. 2 is that aluminic acid zinc-manganese luminescent material prepared by embodiment 3 is the luminescent spectrum comparison diagram under the cathode-ray exciting under 3KV with contrast luminescent material at acceleration voltage; Wherein, curve 1 is the aluminic acid zinc-manganese luminescent material that embodiment 3 makes: the Zn of metal nano particle-doped Ag
0.98al
2o
4: Mn
0.02,
the luminescent spectrum of aluminic acid zinc-manganese luminescent material; Curve 2 is contrast luminescent materials: not metal nano particle-doped Zn
0.98al
2o
4: Mn
0.02the luminescent spectrum of luminescent material.
As can be seen from Figure 2,, at the emission peak at 525nm place, after doping metals, the luminous intensity of luminescent material has strengthened 33% before not adulterating.
Embodiment 4:Zn
0.95al
2o
4: Mn
0.05,
First take alumina aerogels 0.3058g, be dissolved into 6ml and contain Platinic chloride (H
2ptCl
6) 5 × 10
-3in the ethanolic soln of mol/L, at 50 ℃, stir 3h, then ultrasonic 10min, then be dried at 60 ℃, dried sample is ground evenly, precalcining 4h at 600 ℃, obtains the alumina aerogels that contains metal ion.
Take Zn (CH
3cOO)
22H
2o 0.8341g, the Al that contains metal ion
2o
3aerogel 0.4078g, Mn (CH
3cOO)
24H
2o 0.0490g, is placed in agate mortar and is fully ground to and mixes, then by powder transfer in corundum crucible, 1100 ℃ of thermal treatment 10h in retort furnace, then under 1000 ℃ of air atmospheres sintering 6h, be cooled to room temperature, the Zn of the Pt that can obtain adulterating
0.95al
2o
4: Mn
0.05,
luminescent material.
Embodiment 5:Zn
0.94al
2o
4: Mn
0.06,
First take alumina aerogels 0.6117g, be dissolved into 12ml and contain cupric nitrate (Cu (NO
3)
2) 5 × 10
-4in the ethanolic soln of mol/L, at 70 ℃, stir 1h, then ultrasonic 10min, then be dried at 70 ℃, dried sample is ground evenly, precalcining 2h at 800 ℃, obtains the alumina aerogels that contains metal ion.
Take ZnO 0.3126g, the Al that contains metal ion
2o
3aerogel 0.4078g, MnO
20.0207g, is placed in agate mortar and is fully ground to and mixes, then by powder transfer in corundum crucible, 1100 ℃ of thermal treatment 10h in retort furnace, then in tube furnace at pure H
2the lower 1000 ℃ of sintering 6h reduction of reducing atmosphere, is cooled to room temperature, can obtain the Zn of doped with Cu
0.94al
2o
4: Mn
0.06,
luminescent material.
Embodiment 6:Zn
0.9al
2o
4: Mn
0.1,
First take alumina aerogels 0.6117g, be dissolved into 15ml and contain Silver Nitrate (AgNO
3) 5 × 10
-4mol/L and hydrochloro-auric acid (HAuCl
4) 5 × 10
-4in the ethanolic soln of mol/L, at 60 ℃, stir 2h, then ultrasonic 10min, then be dried at 80 ℃, dried sample is ground evenly, precalcining 4h at 1000 ℃, obtains the alumina aerogels that contains metal ion.
Then take Zn (NO
3)
26H
2o 1.0709g, the Al that contains metal ion
2o
3aerogel 0.4078g, Mn (CH
3cOO)
24H
2o 0.0980, is placed in agate mortar and is fully ground to and mixes, then by powder transfer in corundum crucible, 1000 ℃ of thermal treatment 15h in retort furnace, then under 1000 ℃ of air atmospheres sintering 4h, be cooled to room temperature, the Zn of the Ag/Au that can obtain adulterating
0.9al
2o
4: Mn
0.1,
luminescent material.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (10)
1. an aluminic acid zinc-manganese luminescent material, is characterized in that, its general molecular formula is: Zn
1-xal
2o
4: Mn
2+ x, M
y; Wherein, M is metal nano particle-doped, and M is at least one in Ag, Au, Pt, Pd and Cu metal nanoparticle, and the span of x is 0 < x≤0.1, y is the mol ratio of M and Al, and the span of y is 0 < y≤1 × 10-2.
2. aluminic acid zinc-manganese luminescent material according to claim 1, is characterized in that, the span of x is 1 × 10
-3≤ x≤5 × 10
-2, the span of y is 1 × 10
-5≤ y≤5 × 10
-3.
3. aluminic acid zinc-manganese luminescent material according to claim 1, is characterized in that, M is that mol ratio is Ag and the Au of 1: 1.
4. a preparation method for aluminic acid zinc-manganese luminescent material, is characterized in that, comprises the steps:
S1, alumina aerogels is dissolved in the ethanolic soln of M salt, at 50～75 ℃, stir 0.5～3h, then ultrasonic 10min, dry at 60-150 ℃ again, by even dried former abrasive lapping, at 600～1200 ℃, calcine 0.5～4h, make the alumina aerogels that contains M nanoparticle; Wherein, the mol ratio of aluminum oxide and M is less than or equal to 5 × 10 for being greater than 0
-3.
S2, according to general molecular formula Zn
1-xal
2o
4: Mn
2+ x, M
yin the stoichiometric ratio of each element, take the alumina aerogels that includes M nanoparticle making in compound that Zn and Mn are corresponding and step S1, ground and mixed is even, be warming up to 800 ℃～1400 ℃ precalcinings 2～15 hours, in air atmosphere or reducing atmosphere, calcine 0.5～6 hour in 1000 ℃～1400 ℃ again, furnace cooling is cooled to room temperature, and obtained sample is ground to powder, and obtaining general molecular formula is Zn
1-xal
2o
4: Mn
2+ x, M
yaluminic acid zinc-manganese luminescent material;
In above-mentioned steps, M is metal nano particle-doped, and M is at least one in Ag, Au, Pt, Pd and Cu metal nanoparticle, and the span of x is 0 < x≤0.1, y is the mol ratio of M and Al, and the span of y is 0 < y≤1 × 10
-2.
5. the preparation method of aluminic acid zinc-manganese luminescent material according to claim 4, is characterized in that, in step S1, the concentration of the ethanolic soln of M salt is 5 × 10
-6mol/L～1 × 10
-2mol/L.
6. the preparation method of aluminic acid zinc-manganese luminescent material according to claim 4, is characterized in that, in step S2, and at least one in the nitrate of the oxide compound that the compound of Zn is Zn, the carbonate of Zn, Zn, the acetate of Zn and the oxalate of Zn.
7. the preparation method of aluminic acid zinc-manganese luminescent material according to claim 4, is characterized in that, in step S2, and at least one in the nitrate of the oxide compound that the compound of Mn is Mn, the carbonate of Mn, Mn, the acetate of Mn and the oxalate of Mn.
8. the preparation method of aluminic acid zinc-manganese luminescent material according to claim 4, is characterized in that, in step S2, described reducing atmosphere is that volume ratio is the N of 95: 5
2with H
2reducing atmosphere, carbon reducing agent atmosphere or the H of composition
2reducing atmosphere.
9. the preparation method of aluminic acid zinc-manganese luminescent material according to claim 4, is characterized in that, the span of x is 1 × 10
-3≤ x≤5 × 10
-2, the span of y is 1 × 10
-5≤ y≤5 × 10
-3.
10. the preparation method of aluminic acid zinc-manganese luminescent material according to claim 4, is characterized in that, M is that mol ratio is Ag and the Au of 1: 1.
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| CN103710022A (en) * | 2013-11-29 | 2014-04-09 | 佛山安亿纳米材料有限公司 | Light conversion agent, preparation method of light conversion agent, light conversion master batch and preparation method of light conversion master batch |
| CN108728084A (en) * | 2018-05-31 | 2018-11-02 | 陕西科技大学 | A kind of method prepared by porous long after glow luminous material |
| CN110804438A (en) * | 2019-10-15 | 2020-02-18 | 广州大学 | Light color adjustable spinel fluorescent powder and preparation method and application thereof |
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| WO2012000179A1 (en) * | 2010-06-30 | 2012-01-05 | 海洋王照明科技股份有限公司 | Zinc manganese silicate containing metal particles luminescent materials and preparation methods thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710022A (en) * | 2013-11-29 | 2014-04-09 | 佛山安亿纳米材料有限公司 | Light conversion agent, preparation method of light conversion agent, light conversion master batch and preparation method of light conversion master batch |
| CN108728084A (en) * | 2018-05-31 | 2018-11-02 | 陕西科技大学 | A kind of method prepared by porous long after glow luminous material |
| CN110804438A (en) * | 2019-10-15 | 2020-02-18 | 广州大学 | Light color adjustable spinel fluorescent powder and preparation method and application thereof |
| CN110804438B (en) * | 2019-10-15 | 2022-05-10 | 广州大学 | Light color adjustable spinel fluorescent powder and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN103849383B (en) | 2016-12-21 |
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