CN101130691B - Method for improving luminous intensity of vacuum ultraviolet luminescent material with beta-Al2O3 structure - Google Patents

Method for improving luminous intensity of vacuum ultraviolet luminescent material with beta-Al2O3 structure Download PDF

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CN101130691B
CN101130691B CN2007100184077A CN200710018407A CN101130691B CN 101130691 B CN101130691 B CN 101130691B CN 2007100184077 A CN2007100184077 A CN 2007100184077A CN 200710018407 A CN200710018407 A CN 200710018407A CN 101130691 B CN101130691 B CN 101130691B
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purity
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vacuum ultraviolet
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CN101130691A (en
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李峰
王育华
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Nanchang Changrong Mechanical and Electrical Co., Ltd.
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Xian University of Technology
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Abstract

The invention discloses an improving method of vacuum ultraviolet luminous strength with beta-Al2O3 structure, which is characterized by the following: adopting co-doping technique to dop Bi3+, Sb3+ or Zn2+ ion in the vacuum ultraviolet green luminous material with beta-Al2O3 structure; controlling the doping quantity; improving the luminous strength of the vacuum ultraviolet luminous strength with beta-Al2O3 structure, which doesn't has inferior influence for colorful purity of luminous material with simple controlling technique.

Description

Improve and have β-Al 2O 3The method of the luminous intensity of vacuum ultraviolet luminescent material of structure
Technical field
The invention belongs to inorganic embedded photoluminescent material technical field, relate to a kind of employing codoping technology raising and have β-Al 2O 3The method of the luminous intensity of the vacuum ultraviolet luminescent material of structure.
Background technology
A large amount of green luminescent materials that use mainly are Zn in plasma display (PDP) and non-mercury florescent lamp (rare gas lamp) at present 2SiO 4: Mn 2+(ZSM), but Zn 2SiO 4: Mn 2+Discharge characteristic with commonly used PDP redness, blue emitting material very big-difference is arranged, for example red illuminating material uses (Y, Gd) BO 3: Eu 3+, green luminescent material uses Zn 2SiO 4: Mn 2+, blue emitting material uses BaMgAl 10O 17: Eu 2+The time, the phenomenon of having only green pixel cell discharge voltage to uprise can appear.Although can pass through at Zn 2SiO 4: Mn 2+Particle surface carry out coating and improve its discharge characteristic, but will increase Zn like this 2SiO 4: Mn 2+Production cost.In addition, Zn 2SiO 4: Mn 2+Time of persistence longer, its
Figure G2007100184077D00011
1/10 is about 11.9ms.
BaAl 12O 19: Mn 2+With BaMgAl 10O 17: Mn 2+Be two kinds and belong to β-Al 2O 3The vacuum ultraviolet (VUV) green luminescent material of structure is because both crystalline structure, chemical constitution and blue emitting material BaMgAl 10O 17: Eu 2+Similar or identical, therefore there are not the problem of discharge characteristic difference and its purity of color and Zn substantially 2SiO 4: Mn 2+Quite, slightly lack time of persistence (
Figure G2007100184077D00012
1/10 ≈ 6-8ms).Therefore both are considered to substitute the optimal selection of ZSM.But both luminous intensities are compared with ZSM and are still had certain gap, make both applying be subjected to certain obstruction.
The investigator mainly adopts other yuan that mix usually to improve BaAl both at home and abroad 12O 19: Mn 2+And BaMgAl 10O 17: Mn 2+Luminescent properties.The effective co-dopant ions of having reported at present is Mg, Sr, B (Southeast China University's journal, 2005,35:911-914; China's rare-earth journal, 2001,19:586-589; Chinese patent " a kind of aluminate green fluorescent powder of excited by vacuum ultraviolet and manufacture method thereof " (patent No. 01110746.4, open day 2002.11.27, publication number CN1381547) is perhaps by preparation Ba 0.75Al 11O 17.25With the sosoloid of BaMgAl10O17, mix elements (JP patent, 1999,5989455) such as Sr simultaneously, best effect can make luminous intensity than BaAl 12O 19: Mn 2+Improve about 18%.But compare with commercial ZSM and to still have certain gap.Although also can be by codoped Eu2+ as sensitizing agent, doping must be controlled at below the 0.01mol%, otherwise Eu will occur under vacuum ultraviolet-excited 2+Blue-light-emitting, have a strong impact on purity of color (Southeast China University's journal of luminescent material, 2005,35:911-914), and so little doping for present manufacturer for luminescent material high temperature solid-state method commonly used, it is bigger to mix difficulty, therefore still rests on laboratory scale at present, does not have commercialization to use.
Summary of the invention
The purpose of this invention is to provide a kind of raising and have β-Al 2O 3The method of the luminous intensity of vacuum ultraviolet luminescent material of structure not only makes to have β-Al 2O 3The luminous intensity of the vacuum ultraviolet luminescent material of structure is greatly improved, and the purity of color of luminescent material is had no adverse effects.
The technical solution adopted in the present invention is that raising has β-Al 2O 3The method of the luminous intensity of vacuum ultraviolet luminescent material of structure adopts have β-Al 2O 3Codoped ns in the vacuum ultraviolet (VUV) green luminescent material of structure 2Ion.
Characteristics of the present invention also are,
Ns wherein 2Ion is Bi 3+, Sb 3+Or Zn 2+
Bi 3+The ionic doping is: Bi, 0.01～0.25mol%.
Sb 3+The ionic doping is: Sb, 0.01～0.18mol%.
Zn 2+The ionic doping is: Zn, 0.01～0.40mol%.
The invention has the advantages that:
1) compared with prior art, to the material luminous intensity to improve effect more remarkable;
2) doping is moderate, be easy to the commercialization scale production and realize, and raw material sources is extensive, and is cheap, and product cost is not had obvious influence.
3) therefore co-dopant ions has no adverse effects to the luminescent material purity of color at the vacuum ultraviolet-excited visible light that do not send down.
4) technology controlling and process is simple, is suitable for commercialization production.
Description of drawings
Fig. 1 is Bi 3+The X-ray diffraction of doped samples (XRD) figure;
Fig. 2 is Sb 3+The X-ray diffraction of doped samples (XRD) figure;
Fig. 3 is Zn 2+The X-ray diffraction of doped samples (XRD) figure;
Fig. 4 is each dopant ion content and luminous intensity relationship figure;
Fig. 5 is Bi 3+Doping is to the synoptic diagram that influences of colourity;
Fig. 6 is Sb 3+Doping is to the synoptic diagram that influences of colourity;
Fig. 7 is Zn 2+Doping is to the synoptic diagram that influences of colourity.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
Method of the present invention is passed through at BaAl 12O 19: Mn 2+And BaMgAl 10O 17: Mn 2+Deng having β-Al 2O 3Codoped ns in the vacuum ultraviolet (VUV) green luminescent material of structure 2Ion is as Bi 3+, Sb 3+Or Zn 2+, Mn in the material 2+Content be 0.07mol%～0.30mol%, control Bi 3+, Sb 3+Or Zn 2+The ionic doping is respectively: Bi, 0.01～0.25mol%; Sb, 0.01～0.18mol%; Zn, 0.01～0.40mol%.
Embodiment 1
At BaAl 12O 19: Mn 2+Bi mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%); According to chemical formula Ba 0.99Bi 0.01Al 11.9O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1500 ℃ of calcining 4h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 2
At BaAl 12O 19: Mn 2+Bi mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%) is according to chemical formula Ba 0.9Bi 0.1Al 11.9O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H2/95%N 2) in 1400 ℃ of calcining 8h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 3
At BaAl 12O 19: Mn 2+Bi mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%) is according to chemical formula Ba 0.75Bi 0.25Al 11.9O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1600 ℃ of calcining 2h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 4
At BaAl 12O 19: Mn 2+Sb mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Sb 2O 3(purity 99.0%) is according to chemical formula Ba 0.99Sb 0.01Al 11.9O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1500 ℃ of calcining 4h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 5
At BaAl 12O 19: Mn 2+Sb mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Sb 2O 3(purity 99.0%) is according to chemical formula Ba 0.9Sb 0.1Al 11.9O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1400 ℃ of calcining 6h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 6
At BaAl 12O 19: Mn 2+Sb mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Sb 2O 3(purity 99.0%) is according to chemical formula Ba 0.82Sb 0.18Al 11.9O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1600 ℃ of calcining 2h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 7
At BaAl 12O 19: Mn 2+Doping of Zn in the material 2+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), ZnO (purity 99.5%) are according to chemical formula BaZn 0.01Al 11.89O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1500 ℃ of calcining 4h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 8
At BaAl 12O 19: Mn 2+Doping of Zn in the material 2+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), ZnO (purity 99.5%) are according to chemical formula BaZn 0.20Al 11.7O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1400 ℃ of calcining 8h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 9
At BaAl 12O 19: Mn 2+Doping of Zn in the material 2+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), ZnO (purity 99.5%) are according to chemical formula BaZn 0.40Al 11.5O 19: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1600 ℃ of calcining 2h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 10
At BaMgAl 10O 17: Mn 2+Bi mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%) is according to chemical formula Ba 0.99Bi 0.01Mg 0.9Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1500 ℃ of calcining 4h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 11
At BaMgAl 10O 17: Mn 2+Bi mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%) is according to chemical formula Ba 0.9Bi 0.1Mg 0.9Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1600 ℃ of calcining 2h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 12
At BaMgAl 10O 17: Mn 2+Bi mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%) is according to chemical formula Ba 0.75Bi 0.25Mg 0.9Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1400 ℃ of calcining 6h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 13
At BaMgAl 10O 17: Mn 2+Sb mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Sb 2O 3(purity 99.0%) is according to chemical formula Ba 0.99Sb 0.01Mg 0.9Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1400 ℃ of calcining 8h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 14
At BaMgAl 10O 17: Mn 2+Sb mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Sb 2O 3(purity 99.0%) is according to chemical formula Ba 0.9Sb 0.1Mg 0.9Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1500 ℃ of calcining 4h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 15
At BaMgAl 10O 17: Mn 2+Sb mixes in the material 3+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), Bi 2O 3(purity 99.0%), Sb 2O 3(purity 99.0%) and ZnO (purity 99.5%) are according to chemical formula Ba 0.82Sb 0.18Mg 0.9Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1600 ℃ of calcining 2h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 16
At BaMgAl 10O 17: Mn 2+Doping of Zn in the material 2+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), ZnO (purity 99.5%) are according to chemical formula BaZn 0.01Mg 0.89Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1500 ℃ of calcining 4h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 17
At BaMgAl 10O 17: Mn 2+Doping of Zn in the material 2+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), ZnO (purity 99.5%) are according to chemical formula BaZn 0.20Mg 0.70Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1400 ℃ of calcining 8h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Embodiment 18
At BaMgAl 10O 17: Mn 2+Doping of Zn in the material 2+Ion
Choose BaCO 3(purity 99.0%), MgO (purity 99.0%), Al 2O 3(purity 99.99%), MnCO 3(purity 98.5%), ZnO (purity 99.5%) are according to chemical formula BaZn 0.40Mg 0.50Al 10O 17: 0.1Mn 2+Take by weighing the raw material mixed grinding evenly after, at reducing atmosphere (5%H 2/ 95%N 2) in 1600 ℃ of calcining 2h, take out to grind behind the furnace cooling, promptly get the pure white final powdered material of body colour.
Use the D/max-2400 type x-ray powder diffraction instrument of Japan (Rigaku) company of science to carry out test analysis mutually to the thing of the above-mentioned sample that makes; Luminescent properties with FLS920T vacuum ultraviolet (VUV)-visible test system and test sample.
Result by XRD test sees Fig. 1, Fig. 2 and Fig. 3 as can be known, in selected doping scope, and Bi 3+, Sb 3+With Zn 2+Doped samples does not find that all impurity exists mutually.
The test of vacuum ultraviolet (VUV) luminescent properties
Three kinds of ion dopings all effectively raise BaAl 11.9O 19: 0.1Mn 2+Luminous intensity, by Fig. 4 as seen, Bi 3+Make luminous intensity improve 15%, Sb 3+Make luminous intensity improve 35%, Zn 2+Make luminous intensity improve 22%.
By Fig. 5, Fig. 6, Fig. 7 as seen, under the doping condition of luminous intensity the best, three kinds of dopant ions all make purity of color (y value) obtain raising to a certain degree, and this helps the application of luminescent material on display devices such as PDP.

Claims (1)

1. improve and have β-Al 2O 3The method of the luminous intensity of vacuum ultraviolet luminescent material of structure is characterized in that, has BaAl 12O 19: Mn 2+The vacuum ultraviolet (VUV) green luminescent material in codoped Bi 3+, Sb 3+Or Zn 2+Ion, described Bi 3+The ionic doping is according to chemical formula Ba 0.99Bi 0.01Al 11.9O 19: 0.1Mn 2+Take by weighing, perhaps according to chemical formula Ba 0.9Bi 0.1Al 11.9O 19: 0.1 Mn 2+Take by weighing, perhaps according to chemical formula Ba 0.75Bi 0.25Al 11.9O 19: 0.1 Mn 2+Take by weighing; Described Sb 3+The ionic doping is according to chemical formula Ba 0.99Sb 0.01Al 11.9O 19: 0.1 Mn 2+Take by weighing, perhaps according to chemical formula Ba 0.9Sb 0.1Al 11.9O 19: 0.1 Mn 2+Take by weighing, perhaps according to chemical formula Ba 0.82Sb 0.18Al 11.9O 19: 0.1 Mn 2+Take by weighing; Described Zn 2+The ionic doping is according to chemical formula BaZn 0.01Al 11.89O 19: 0.1 Mn 2+Take by weighing, perhaps according to chemical formula BaZn 0.20Al 11.7O 19: 0.1Mn 2+Take by weighing, perhaps according to chemical formula BaZn 0.40Al 11.5O 19: 0.1Mn 2+Take by weighing.
CN2007100184077A 2007-08-03 2007-08-03 Method for improving luminous intensity of vacuum ultraviolet luminescent material with beta-Al2O3 structure Expired - Fee Related CN101130691B (en)

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CN102391860A (en) * 2011-09-28 2012-03-28 陕西科技大学 Rare earth europium-doped alumina fiber luminous material and preparation method thereof
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Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1366017A (en) * 2002-03-15 2002-08-28 中国科学院长春应用化学研究所 Vacuum ultraviolet ray excited green barium magnesium aluminate as fluorescent substance and its preparing process
US6454967B1 (en) * 1999-11-04 2002-09-24 Samsung Sdi Co., Ltd. Green-emitting phosphors for plasma display panel and preparing method thereof
CN1660963A (en) * 2003-11-20 2005-08-31 三星Sdi株式会社 Green light-emitting phosphor for vacuum ultraviolet-excited light-emitting device, light-emitting device including the same, and method of preparing the same
CN1219848C (en) * 2001-04-19 2005-09-21 北京有色金属研究总院 Vacuum ultraviolet excited green aluminate fluorescent powder and its preparing process

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
US6454967B1 (en) * 1999-11-04 2002-09-24 Samsung Sdi Co., Ltd. Green-emitting phosphors for plasma display panel and preparing method thereof
CN1219848C (en) * 2001-04-19 2005-09-21 北京有色金属研究总院 Vacuum ultraviolet excited green aluminate fluorescent powder and its preparing process
CN1366017A (en) * 2002-03-15 2002-08-28 中国科学院长春应用化学研究所 Vacuum ultraviolet ray excited green barium magnesium aluminate as fluorescent substance and its preparing process
CN1660963A (en) * 2003-11-20 2005-08-31 三星Sdi株式会社 Green light-emitting phosphor for vacuum ultraviolet-excited light-emitting device, light-emitting device including the same, and method of preparing the same

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