CN101358132B - Rare-earth red luminous material for plasma panel display and non-mercury fluorescent lamp and preparing process thereof - Google Patents

Rare-earth red luminous material for plasma panel display and non-mercury fluorescent lamp and preparing process thereof Download PDF

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Publication number
CN101358132B
CN101358132B CN2008101986135A CN200810198613A CN101358132B CN 101358132 B CN101358132 B CN 101358132B CN 2008101986135 A CN2008101986135 A CN 2008101986135A CN 200810198613 A CN200810198613 A CN 200810198613A CN 101358132 B CN101358132 B CN 101358132B
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rare earth
rare
earth
red
agate mortar
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CN101358132A (en
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梁宏斌
韩冰
钟玖平
田梓峰
苏锵
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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Abstract

The present invention discloses a rear-earth red-light-emitting material used for plasma display panels (PDP) and mercury-free fluorescent lamps. The expression of the chemical composition of the rear-earth red-light-emitting material is as follows: M(RE[1-x]Eux)(PO3)4; wherein, M is alkali metal ion selected from Li<+>, Na<+>, K<+>, Rb<+> and Cs<+>; RE is a rear earth element selected from La<3+>, Gd<3+>, Y<3+> and Lu<3+>; Eu<3+> is an active ion; and x is the molar percentage content of luminous active ions relative to RE atoms ranging: 0.01<= x <= 1.0. The preparation method is simple, and the prepared rear-earth red-light-emitting material used for PDPs and mercury-free fluorescent lamps is activated by vacuum ultraviolet (VUV) light to emit strong red light at 590nm, which is stronger than the red light emitted by the red fluorescent powder (Y, Gd)BO3 : Eu<3+> used in the prior plasma display panels, approximately 110 percent of the red light.

Description

A kind of plasma flat shows and non-mercury florescent lamp rare-earth red luminous material and preparation method thereof
Technical field
The present invention relates to a kind of PDP (plasma flat demonstration) rare earth luminescent material and preparation method thereof.
Background technology
Plasma flat-plate shows that (plasma display panels is called for short PDP) can be made into the indicating meter of large-size; it is the optimal selection of wall hung television; and non-mercury florescent lamp does not contain the deleterious mercury of human body owing to it; compare and traditional high voltage mercury lamp and low pressure mercury lamp, have great importance from the environment protection angle.Therefore, the research of the three primary colors fluorescent powder that PDP and non-mercury florescent lamp are used is most important.
PDP and non-mercury florescent lamp are with being work under vacuum ultraviolet photon (VUV) radiation of 100-200nm scope, the energy of VUV photon is according to the 254nm shortwave UV in the source, Mingguang City and the energy height of 365nm long wave UV photon, thereby the fluorescent material that PDP uses is had particular requirement: (1) is the luminous efficiency height under the VUV photon excitation; (2) bombardment of anti-high-energy photon, light decay is little, long working life; (3) twilight sunset satisfies the requirement of technique of display, below 10ms; (4) the chromaticity coordinates value meets the demands, high color purity, and colour gamut is wide; (5) granular size is suitable; (6) stable chemical performance is not decomposed during work.
It is relatively good to be considered to effect at present, and the fluorescent material that reaches commercial applications has red Y 2O 3: Eu, (Y, Gd) BO 3: Eu, green Zn 2SiO 4: Mn, BaAl 12O 19: Mn and blue BaMgAl 10O 17: Eu, they the time similar fluorescent material in fluorescence quantum efficiency than higher, their fluorescence quantum efficiency is all more than 1.0.But used red bluish-green three primary colors fluorescent powder also exists problem in actual applications now, and luminous efficiency and luminous efficiency are low during common ground.Red-emitting phosphors (Y, Gd) BO 3: Eu compares Y 2O 3: Eu efficient height, but it luminously mainly is 5D 0- 7F 1Magnetic dipole transition, main emission peak is the 593nm of transition emission, and is luminous than main peak more orange at 611nm.And the twilight sunset of green-emitting phosphor oversize (12.5ms) is too wide in the gap with ideal 1-5ms time of persistence, the requirement that is unsuitable for showing.Activated blue aluminate fluor mainly is that thermostability and anti-VUV radiation capacity are poor.Therefore, for the development that adapts to demonstration and the needs of green illumination, we should seek new material system, solve existing variety of issue, make fluorescent material can satisfy the requirement of use.
Summary of the invention
The purpose of this invention is to provide a kind of PDP and non-mercury florescent lamp rare-earth red luminous material with strong red emission.
Another object of the present invention provides the preparation method of above-mentioned rare-earth red luminous material.
PDP of the present invention and non-mercury florescent lamp have following chemical constitution expression with rare-earth red luminous material: M (RE 1-xEu x) (PO 3) 4, wherein, M is an alkalimetal ion, is selected from Li +, Na +, K +, Rb +, Cs +RE is a rare earth element, is selected from La 3+, Gd 3+, Y 3+, Lu 3+Eu 3+(trivalent rare earth europium ion) is active ions; X is activation ion (europium ion) the shared molar content of RE atom relatively, span: 0.01≤x≤1.0.
The selected substrate material of the present invention is basic metal rare earth tetrametaphosphate [MRE (PO 3) 4].Luminescence center is trivalent rare earth europium ion (Eu 3+).Under vacuum ultraviolet (VUV) (VUV) optical excitation, trivalent rare earth europium ion (Eu 3+) send ruddiness.
Among the present invention, trivalent europium ion activated plasma flat-plate shows (PDP) and non-mercury florescent lamp, and method is synthetic mutually with the traditional high reviewing knowledge already acquired of rare earth tetrametaphosphate powder employing, and preparation technology is simple, easy handling, and equipment is easy to get, operational safety, condition is controlled easily.
Raw material of the present invention can resolve into the alkaline carbonate of alkalimetal oxide, the mixture of one or more of base metal nitrate when being heating; Can resolve into the rare-earth oxalate of rare earth oxide when rare earth oxide or heating, rare earth carbonate, the mixture of one or more in the rare earth nitrate; Can resolve into the ammonium di-hydrogen phosphate of Vanadium Pentoxide in FLAKES when Vanadium Pentoxide in FLAKES or heating, the mixture of one or more in the DAP etc.
Raw material is pressed the accurate weighing of chemical constitution formula, mix, put into process furnace then, 300 ℃～800 ℃ following calcination at least 2 hours, treat to take out behind the furnace temperature naturally cooling, promptly obtain trivalent europium ion activated plasma flat-plate after the pulverizing and show and the rare earth luminous powder of non-mercury florescent lamp.
Compared with prior art, the present invention has following beneficial effect: preparation method of the present invention is simple, prepared PDP and non-mercury florescent lamp use rare-earth red luminous material under vacuum ultraviolet (VUV) (VUV) optical excitation, there is strong ruddiness to send at the 590nm place, show method red light fluorescent powder (Y, Gd) BO that uses in the phase device than present plasma flat-plate 3: Eu 3+Stronger red emission is arranged, be approximately 110% of its intensity.
Description of drawings
(a is under difference monitoring launching condition b) to last figure among Fig. 1, the excitation spectrum contrast figure of the material that glows (b) that uses in the rare-earth red luminous material of embodiment 1 (a) and the present plasma panel display spare;
(c is under the same vacuum ultraviolet (VUV) optical excitation d) to figure below among Fig. 1, the emmission spectrum contrast figure of the material that glows (d) that uses in the rare-earth red luminous material of embodiment 1 (c) and the present plasma panel display spare.
Embodiment
Embodiment 1
Take by weighing Carbon Dioxide lithium (Li 2CO 3) 0.0739g, europium sesquioxide (Eu 2O 3) 0.3519g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 30 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Measure plasma flat of the present invention and show that (PDP) and non-mercury florescent lamp are with the rare earth excitation spectrum of material under 590nm monitors that glow, find that this luminescent material all has stronger absorption at 147nm and 172nm place, the master that is absorbed as with the 172nm place, the light absorbing wavelength that shows this luminescent material at vacuum ultraviolet, the basic rare gas mixed gas plasma of xenon (Xe) that extensively adopts with present plasma panel display spare and non-mercury florescent lamp produce the vacuum ultraviolet (VUV) optical wavelength coincide better, can realize efficiently exciting in PDP and the non-mercury florescent lamp device.Fig. 1 (a), Fig. 1 (b) have provided the vacuum ultraviolet-excited spectrum under monitoring 590nm launching condition and the emmission spectrum of this luminescent material under 172nm excites respectively.As a comparison, use in the plasma panel display spare at present red phosphor (Y, Gd) BO 3: Eu 3+Under monitoring 592nm launching condition vacuum ultraviolet-excited spectrum and the emmission spectrum under the optical excitation of 172nm vacuum ultraviolet (VUV) be shown in Fig. 1 (c) and Fig. 1 (d) respectively.Emmission spectrum by two kinds of fluorescent material of integration can draw, the integral area of the emmission spectrum of fluorescent material of the present invention is 44, and the integral area of the emmission spectrum of commercial fluorescent material is 39, this that is to say, plasma flat of the present invention shows that (PDP) and non-mercury florescent lamp are glow material (Y, Gd) BO of commercialization with the glow emissive porwer of material of rare earth 3: Eu 3+110%, improved about 10% from luminous intensity.
Embodiment 2
Take by weighing anhydrous sodium carbonate (Na 2CO 3) 0.1060g, europium sesquioxide (Eu 2O 3) 0.3519g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 30 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 3
Take by weighing Anhydrous potassium carbonate (K 2CO 3) 0.1382g, europium sesquioxide (Eu 2O 3) 0.3519g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 30 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 4
Take by weighing Carbon Dioxide caesium (Cs 2CO 3) 0.3258g, europium sesquioxide (Eu 2O 3) 0.3519g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 30 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 5
Take by weighing Carbon Dioxide lithium (Li 2CO 3) 0.0739g, europium sesquioxide (Eu 2O 3) 0.3167g, gadolinium sesquioxide (Gd 2O 3) 0.0362g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 6 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 6
Take by weighing anhydrous sodium carbonate (Na 2CO 3) 0.1060g, europium sesquioxide (Eu 2O 3) 0.3167g, gadolinium sesquioxide (Gd 2O 3) 0.0362g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 6 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 7
Take by weighing Anhydrous potassium carbonate (K 2CO 3) 0.1382g, europium sesquioxide (Eu 2O 3) 0.3167g, gadolinium sesquioxide (Gd 2O 3) 0.0362g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 6 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 8
Take by weighing Carbon Dioxide caesium (Cs 2CO 3) 0.3258g, europium sesquioxide (Eu 2O 3) 0.3167g, gadolinium sesquioxide (Gd 2O 3) 0.0362g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 6 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 9
Take by weighing Carbon Dioxide lithium (Li 2CO 3) 0.0739g, europium sesquioxide (Eu 2O 3) 0.3167g, yttrium oxide (Y 2O 3) 0.0226g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 10
Take by weighing anhydrous sodium carbonate (Na 2CO 3) 0.1060g, europium sesquioxide (Eu 2O 3) 0.3167g, yttrium oxide (Y 2O 3) 0.0226g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 11
Take by weighing Anhydrous potassium carbonate (K 2CO 3) 0.1382g, europium sesquioxide (Eu 2O 3) 0.3167g, yttrium oxide (Y 2O 3) 0.0226g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 12
Take by weighing Carbon Dioxide caesium (Cs 2CO 3) 0.3258g, europium sesquioxide (Eu 2O 3) 0.3167g, yttrium oxide (Y 2O 3) 0.0226g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 13
Take by weighing Carbon Dioxide lithium (Li 2CO 3) 0.0739g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 14
Take by weighing anhydrous sodium carbonate (Na 2CO 3) 0.1060g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 15
Take by weighing Anhydrous potassium carbonate (K 2CO 3) 0.1382g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 16
Take by weighing Carbon Dioxide caesium (Cs 2CO 3) 0.3258g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 17
Take by weighing Carbon Dioxide lithium (Li 2CO 3) 0.0739g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 18
Take by weighing anhydrous sodium carbonate (Na 2CO 3) 0.1060g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 19
Take by weighing Anhydrous potassium carbonate (K 2CO 3) 0.1382g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 20
Take by weighing Carbon Dioxide caesium (Cs 2CO 3) 0.3258g, europium sesquioxide (Eu 2O 3) 0.3167g, lanthanum trioxide (La 2O 3) 0.0326g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 700 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 21
Take by weighing Carbon Dioxide lithium (Li 2CO 3) 0.0739g, europium sesquioxide (Eu 2O 3) 0.3167g, lutecium oxide (Lu 2O 3) 0.0398g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 750 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 22
Take by weighing anhydrous sodium carbonate (Na 2CO 3) 0.1060g, europium sesquioxide (Eu 2O 3) 0.3167g, lutecium oxide (Lu 2O 3) 0.0398g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 750 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 23
Take by weighing Anhydrous potassium carbonate (K 2CO 3) 0.1382g, europium sesquioxide (Eu 2O 3) 0.3167g, lutecium oxide (Lu 2O 3) 0.0398g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 750 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.
Embodiment 24
Take by weighing Carbon Dioxide caesium (Cs 2CO 3) 0.3258g, europium sesquioxide (Eu 2O 3) 0.3167g, lutecium oxide (Lu 2O 3) 0.0398g, ammonium di-hydrogen phosphate (NH 4H 2PO 4) 0.9202g, after fully grinding in agate mortar and mixing, 750 ℃ are incubated 10 hours, drop to room temperature naturally, take out, and after grinding in agate mortar, obtain the finished product.

Claims (2)

1. a plasma flat shows and the non-mercury florescent lamp rare-earth red luminous material its chemical constitution expression: M (RE 1-xEu x) (PO 3) 4, wherein, M is an alkalimetal ion, is selected from Li +, Na +, K +, Rb +, Cs +RE is a rare earth element, is selected from La 3+, Gd 3+, Y 3+, Lu 3+Eu 3+Be active ions; X is the shared molar content of the relative RE atom of activation ion, span: 0.01≤x≤1.0.
2. the described plasma flat of claim 1 shows and the glow preparation method of rare earth luminescent material of non-mercury florescent lamp usefulness, it is characterized in that comprising the steps: with raw material by the accurate weighing of chemical constitution formula, mix, putting into process furnace then calcines, treat to take out behind the furnace temperature naturally cooling, promptly obtain trivalent europium ion activated plasma flat-plate after the pulverizing and show and the rare earth luminous powder of non-mercury florescent lamp;
Described raw material the time can resolve into one or more mixture of alkaline carbonate, the base metal nitrate of alkalimetal oxide for heating; Rare earth oxide or heating the time can be resolved into one or more the mixture in the rare-earth oxalate, rare earth carbonate, rare earth nitrate of rare earth oxide; Vanadium Pentoxide in FLAKES or heating the time can be resolved into the ammonium di-hydrogen phosphate of Vanadium Pentoxide in FLAKES, one or more the mixture in the DAP;
Described calcining temperature is 300 ℃～800 ℃, and calcination time is 2～30 hours.
CN2008101986135A 2008-09-18 2008-09-18 Rare-earth red luminous material for plasma panel display and non-mercury fluorescent lamp and preparing process thereof Expired - Fee Related CN101358132B (en)

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CN102199429B (en) * 2010-03-24 2014-05-07 海洋王照明科技股份有限公司 Fluophosphate-based light-emitting material and preparation method thereof
CN102899046B (en) * 2011-07-26 2015-11-25 比亚迪股份有限公司 A kind of red fluorescence powder and preparation method thereof
CN102585817A (en) * 2011-12-31 2012-07-18 四川虹欧显示器件有限公司 Red fluorescent powder for PDP (Plasma Display Panel) and preparation method thereof
CN103289698B (en) * 2013-06-27 2015-10-28 苏州大学 A kind of europium ion Eu 3+the phosphate base red fluorescence powder activated, preparation method and application
CN109266345A (en) * 2018-10-29 2019-01-25 江苏师范大学 A kind of single matrix phosphate white emitting fluorescent powder of rare earth ion codope and preparation method thereof

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