CN102337129A - Red luminescent fluorescent powder for FED (Field Emission Display) and preparation method thereof - Google Patents
Red luminescent fluorescent powder for FED (Field Emission Display) and preparation method thereof Download PDFInfo
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- CN102337129A CN102337129A CN2011102058037A CN201110205803A CN102337129A CN 102337129 A CN102337129 A CN 102337129A CN 2011102058037 A CN2011102058037 A CN 2011102058037A CN 201110205803 A CN201110205803 A CN 201110205803A CN 102337129 A CN102337129 A CN 102337129A
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Abstract
The invention discloses red luminescent fluorescent powder for a FED (Field Emission Display) and a preparation method thereof. The fluorescent powder is coactivated by europium and terbium and has a mass ratio of yttrium oxide to europium oxide to terbium oxide of (92 to 97):(2.5 to 7.5):(0.001 to 0.005). The red luminescent fluorescent powder for the FED, which is provided by the invention, is the yttrium oxide coactivated by europium and terbium. Compared with the existing yttrium oxide europium fluorescent powder for the FED,which is activated by europium, under the same conditions of a spectrum, chromaticity and granularity, the yttrium oxide europium terbium fluorescent powder for the FED, which is coactivated by europium terbium, has higher brightness and has the advantage of high stability in the application process.
Description
Technical field
The invention belongs to FED and use the fluorescent material technical field, relate to a kind of FED with red luminescence phosphor and preparation method thereof.
Background technology
At present, FED is mainly the yttrium europium oxide red fluorescence powder with red luminescence phosphor, and the yttrium europium oxide red fluorescence powder is europkium-activated, and firing temperature is generally at 1300～1380 ℃.But on high-quality FED, there is the shortcoming of low lightness in this fluorescent material.
Summary of the invention
The problem that the present invention solves is to provide a kind of FED with red luminescence phosphor and preparation method thereof, through the co-activation of europium and terbium, improves the luminosity and the stability of red luminescence phosphor.
The present invention realizes through following technical scheme:
A kind of FED uses red luminescence phosphor, and this fluorescent material is the coactivated fluorescent material of europium and terbium, by quality ratio, and yttrium oxide: europium sesquioxide: terbium sesquioxide=(92～97): (2.5～7.5): (0.001～0.005).
By quality ratio, yttrium oxide: europium sesquioxide: terbium sesquioxide=(92.55～96.55): (3.45～7.45): (0.002～0.003).
A kind of FED may further comprise the steps with the preparation method of red luminescence phosphor:
1) according to yttrium oxide: europium sesquioxide: terbium sesquioxide=(92～97): (2.5～7.5): the mass ratio of (0.001～0.005); With yttrium oxide, europium sesquioxide, terbium sesquioxide thorough mixing; And then add the bariumchloride of mixing back quality 1.5～3.5% and 0.10～0.15% boric acid thorough mixing, obtain the fluorescence powder;
2) the fluorescence powder is packed in the airtight container, at 1200～1500 ℃ of following heat preservation sintering 4～6h;
3) fluorescent material that burns till is taken out the back and pulverize, wet method is dispersed into slurry, is disperseing to cross simultaneously 100～200 eye mesh screens, and fluorescent material is collected in dehydration then;
4) fluorescent material of collecting that will dewater disperses in dispersion machine, and the fluorescent material water flushing that clears branch is down through 300～500 eye mesh screens, then with fluorescent material with water washing 6～9 times, wash churning time 15～30min, the fluorescent material of dehydration collection at last at every turn;
5) the fluorescent material that has dewatered dry 4～24h under 100～150 ℃; Cross 300～500 eye mesh screens to the good fluorescent material of drying, obtain FED and use red luminescence phosphor.
The thorough mixing of described yttrium oxide, europium sesquioxide, terbium sesquioxide is that it is processed the heavy altogether article of yttrium europium oxide terbium that granularity is 3.0～5.0 μ m in proportion, and then adds the yttrium europium oxide terbium and sink the bariumchloride of quality 1.5～3.5% and 0.10～0.15% boric acid thorough mixing altogether.
Being mixed into of described fluorescence powder:, in mixer, mix 60～120min afterwards with mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding.
Described bariumchloride also carries out following pre-treatment: with bariumchloride 3～6h when descending drying for 100～130 ℃.
Described airtight container be airtight alumina crucible.
The described fluorescent material collected of will dewatering disperses in liner is the dispersion machine of ceramic tile; Dispersion condition is 2～3 times of the fluorescent material quality, the dispersion glass sphere of diameter 2.5～5mm; Water consumption is 1～3 times of fluorescent material quality, and the dispersion rotating speed is 1.5～4.0r/min, jitter time 1.5～3h.
It is to carry out centrifuge dehydration with whizzer that fluorescent material is collected in said dehydration.
Compared with prior art, the present invention has following beneficial technical effects:
FED provided by the invention uses red luminescence phosphor, is the co-activation yttrium oxide through europium and terbium.Compare with the fluorescent material of europkium-activated yttrium europium oxide with present FED, under spectrum and colourity and granularity the same terms, the coactivated yttrium europium oxide terbium fluorescent material through europium and terbium has higher luminosity, in application process, has the high advantage of stability.
Description of drawings
Fig. 1 is the micro-view of particle (* 5000) of the yttrium europium oxide terbium red luminescence phosphor of the present invention's preparation;
Fig. 2 is the micro-view of particle (* 10000) of the yttrium europium oxide terbium red luminescence phosphor of the present invention's preparation;
Fig. 3 is the stimulated luminescence spectrogram of the yttrium europium oxide terbium red luminescence phosphor of the present invention's preparation; X-coordinate is the wavelength that excites, and ordinate zou is a luminosity.
Embodiment
Below in conjunction with concrete embodiment the present invention is done further detailed description, said is to explanation of the present invention rather than qualification.
Embodiment 1
FED may further comprise the steps with the preparation method of red luminescence phosphor:
1) the solubility promoter bariumchloride is dry: solubility promoter bariumchloride (molecular formula BaCl
22H
2O) in electric drying apparatus, carry out drying and anhydrate, drying conditions is that drying temperature is that 120 ± 5 ℃, time of drying are 3～6Hr, and dry intact back is contained in the solubility promoter bariumchloride in the Plastic Bottle that out-of-the-way light seals for use;
In massfraction, with the yttrium oxide amount be 96.547%, the europium sesquioxide amount is 3.45%, the terbium sesquioxide amount is 0.003% to grind the back thorough mixing, and then adds bariumchloride and boric acid mixes; The solubility promoter bariumchloride amount of quoting be the blended quality 1.5%, the solubility promoter boric acid amount of quoting is 0.15% of blended quality;
Perhaps; For with yttrium oxide, europium sesquioxide, terbium sesquioxide better mixing; According to the preparation method of heavy article altogether (can with reference to the yttrium europium oxide preparation of heavy article altogether), the yttrium europium oxide terbium that prepare the yttrium oxide amount and be 96.547%, the europium sesquioxide amount is 3.45%, the terbium sesquioxide amount is 0.003% (in massfraction) sinks article altogether; With mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding, in mixer, mix 120min afterwards, obtain the fluorescence powder; The solubility promoter bariumchloride amount of quoting be the heavy altogether quality of yttrium europium oxide terbium 1.5%, the solubility promoter boric acid amount of quoting be the yttrium europium oxide terbium altogether heavy quality 0.15%.
2) with the fluorescence powder that the prepares 0.5kg that in alumina crucible, packs into, it is flat to shake, and covers alumina crucible completely with alumina cover; Burning till 1400 ℃ of firing temperatures in the electric stove in self acting tunnel continuously; Firing time 6h;
3) take out collection to burned fluorescent material; Pulverize with Hubei Province formula dispersion machine earlier, morcel machine with roll-type afterwards and pulverize; Under the flushing of pure water, sieve the fluorescent material that crushes through 200 order nylon screens, the powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering;
4) in liner is the dispersion machine of ceramic tile, disperse the fluorescent material that has taken off water, dispersion condition is that the dispersion glass sphere consumption of diameter 2.5mm is that 2 times of the fluorescent material quality, pure water consumption are 1 times of the fluorescent material quality, disperse 2.0 rev/mins of rotating speeds, jitter time 3 hours;
5) fluorescent material that clears branch sieves through 500 order nylon screens under the flushing of pure water; Wash the fluorescent material that branch clears, the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
The powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering; Put into the inherent electricity of fine aluminium plate to the fluorescent material that has dewatered or steam dryer carries out drying, drying temperature is that 120 ℃, time of drying are 10Hr;
The fluorescent material good drying sieves with 500 order nylon screens, obtains FED and uses red luminescence phosphor.
Embodiment 2
FED may further comprise the steps with the preparation method of red luminescence phosphor:
1) the solubility promoter bariumchloride is dry: solubility promoter bariumchloride (molecular formula BaCl
22H
2O) in electric drying apparatus, carry out drying and anhydrate, drying conditions is that drying temperature is that 110 ± 5 ℃, time of drying are 3～6Hr, and dry intact back is contained in the solubility promoter bariumchloride in the Plastic Bottle that out-of-the-way light seals for use;
Prepare the yttrium europium oxide terbium according to the preparation method of heavy article altogether and sink article altogether, wherein, the yttrium oxide amount is 95.547%, the europium sesquioxide amount is 4.45%, the terbium sesquioxide amount is 0.003%; The solubility promoter bariumchloride amount of quoting be the heavy altogether quality of yttrium europium oxide terbium 3.0%, the solubility promoter boric acid amount of quoting be the yttrium europium oxide terbium altogether heavy quality 0.10%;
With mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding, in mixer, mix 120min afterwards, obtain the fluorescence powder.
2) with the fluorescence powder that the prepares 0.5kg that in alumina crucible, packs into, it is flat to shake, and covers alumina crucible completely with alumina cover; Burning till 1430 ℃ of firing temperatures in the electric stove in self acting tunnel continuously; Firing time 5h;
3) take out collection to burned fluorescent material; Pulverize with Hubei Province formula dispersion machine earlier, morcel machine with roll-type afterwards and pulverize; Under the flushing of pure water, sieve the fluorescent material that crushes through 200 order nylon screens, the powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering;
4) in liner is the dispersion machine of ceramic tile, disperse the fluorescent material that has taken off water, dispersion condition is that the dispersion glass sphere consumption of diameter 2.5mm is that 2 times of the fluorescent material quality, pure water consumption are 1 times of the fluorescent material quality, disperse 2.0 rev/mins of rotating speeds, jitter time 3 hours;
5) fluorescent material that clears branch sieves through 500 order nylon screens under the flushing of pure water; Wash the fluorescent material that branch clears, the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
The powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering; Put into the inherent electricity of fine aluminium plate to the fluorescent material that has dewatered or steam dryer carries out drying, drying temperature is that 120 ℃, time of drying are 10Hr;
The fluorescent material good drying sieves with 500 order nylon screens, obtains FED and uses red luminescence phosphor.
Embodiment 3
FED may further comprise the steps with the preparation method of red luminescence phosphor:
1) the solubility promoter bariumchloride is dry: solubility promoter bariumchloride (molecular formula BaCl
22H
2O) in electric drying apparatus, carry out drying and anhydrate, drying conditions is that drying temperature is that 110 ± 5 ℃, time of drying are 3～6Hr, and dry intact back is contained in the solubility promoter bariumchloride in the Plastic Bottle that out-of-the-way light seals for use;
Prepare the yttrium europium oxide terbium according to the preparation method of heavy article altogether and sink article altogether, wherein, the yttrium oxide amount is 92.548%, the europium sesquioxide amount is 7.45%, the terbium sesquioxide amount is 0.002%; The solubility promoter bariumchloride amount of quoting be the heavy altogether quality of yttrium europium oxide terbium 2.0%, the solubility promoter boric acid amount of quoting be the yttrium europium oxide terbium altogether heavy quality 0.14%;
With mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding, in mixer, mix 120min afterwards, obtain the fluorescence powder.
2) with the fluorescence powder that the prepares 0.5kg that in alumina crucible, packs into, it is flat to shake, and covers alumina crucible completely with alumina cover; Burning till 1390 ℃ of firing temperatures in the electric stove in self acting tunnel continuously; Firing time 5h;
3) take out collection to burned fluorescent material; Pulverize with Hubei Province formula dispersion machine earlier, morcel machine with roll-type afterwards and pulverize; Under the flushing of pure water, sieve the fluorescent material that crushes through 200 order nylon screens, the powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering;
4) in liner is the dispersion machine of ceramic tile, disperse the fluorescent material that has taken off water, dispersion condition is that the dispersion glass sphere consumption of diameter 2.5mm is that 2 times of the fluorescent material quality, pure water consumption are 1 times of the fluorescent material quality, disperse 2.0 rev/mins of rotating speeds, jitter time 3 hours;
5) fluorescent material that clears branch sieves through 500 order nylon screens under the flushing of pure water; Wash the fluorescent material that branch clears, the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
The powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering; Put into the inherent electricity of fine aluminium plate to the fluorescent material that has dewatered or steam dryer carries out drying, drying temperature is that 120 ℃, time of drying are 10Hr;
The fluorescent material good drying sieves with 500 order nylon screens, obtains FED and uses red luminescence phosphor.
Embodiment 4
FED may further comprise the steps with the preparation method of red luminescence phosphor:
1) the solubility promoter bariumchloride is dry: solubility promoter bariumchloride (molecular formula BaCl
22H
2O) in electric drying apparatus, carry out drying and anhydrate, drying conditions is that drying temperature is that 110 ± 5 ℃, time of drying are 3～6Hr, and dry intact back is contained in the solubility promoter bariumchloride in the Plastic Bottle that out-of-the-way light seals for use;
Prepare the yttrium europium oxide terbium according to the preparation method of heavy article altogether and sink article altogether, wherein, the yttrium oxide amount is 95.445%, the europium sesquioxide amount is 4.55%, the terbium sesquioxide amount is 0.005%; The solubility promoter bariumchloride amount of quoting be the heavy altogether quality of yttrium europium oxide terbium 2.5%, the solubility promoter boric acid amount of quoting be the yttrium europium oxide terbium altogether heavy quality 0.12%;
With mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding, in mixer, mix 60min afterwards, obtain the fluorescence powder.
2) with the fluorescence powder that the prepares 0.5kg that in alumina crucible, packs into, it is flat to shake, and covers alumina crucible completely with alumina cover; Burning till 1450 ℃ of firing temperatures in the electric stove in self acting tunnel continuously; Firing time 4h;
3) take out collection to burned fluorescent material; Pulverize with Hubei Province formula dispersion machine earlier, morcel machine with roll-type afterwards and pulverize; Under the flushing of pure water, sieve the fluorescent material that crushes through 200 order nylon screens, the powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering;
4) in liner is the dispersion machine of ceramic tile, disperse the fluorescent material that has taken off water, dispersion condition is that the dispersion glass sphere consumption of diameter 2.5mm is that 2 times of the fluorescent material quality, pure water consumption are 1 times of the fluorescent material quality, disperse 2.0 rev/mins of rotating speeds, jitter time 3 hours;
5) fluorescent material that clears branch sieves through 500 order nylon screens under the flushing of pure water; Wash the fluorescent material that branch clears, the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
The powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering; Put into the inherent electricity of fine aluminium plate to the fluorescent material that has dewatered or steam dryer carries out drying, drying temperature is that 120 ℃, time of drying are 10Hr;
The fluorescent material good drying sieves with 500 order nylon screens, obtains FED and uses red luminescence phosphor.
Embodiment 5
FED may further comprise the steps with the preparation method of red luminescence phosphor:
1) the solubility promoter bariumchloride is dry: solubility promoter bariumchloride (molecular formula BaCl
22H
2O) in electric drying apparatus, carry out drying and anhydrate, drying conditions is that drying temperature is that 110 ± 5 ℃, time of drying are 3～6Hr, and dry intact back is contained in the solubility promoter bariumchloride in the Plastic Bottle that out-of-the-way light seals for use;
Prepare the yttrium europium oxide terbium according to the preparation method of heavy article altogether and sink article altogether, wherein, the yttrium oxide amount is 93.44%, the europium sesquioxide amount is 6.559%, the terbium sesquioxide amount is 0.001%; The solubility promoter bariumchloride amount of quoting be the heavy altogether quality of yttrium europium oxide terbium 3.5%, the solubility promoter boric acid amount of quoting be the yttrium europium oxide terbium altogether heavy quality 0.10%;
With mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding, in mixer, mix 80min afterwards, obtain the fluorescence powder.
2) with the fluorescence powder that the prepares 0.5kg that in alumina crucible, packs into, it is flat to shake, and covers alumina crucible completely with alumina cover; Burning till 1250 ℃ of firing temperatures in the electric stove in self acting tunnel continuously; Firing time 4h;
3) take out collection to burned fluorescent material; Pulverize with Hubei Province formula dispersion machine earlier, morcel machine with roll-type afterwards and pulverize; Under the flushing of pure water, sieve the fluorescent material that crushes through 200 order nylon screens, the powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering;
4) in liner is the dispersion machine of ceramic tile, disperse the fluorescent material that has taken off water, dispersion condition is that the dispersion glass sphere consumption of diameter 3.5mm is that 3 times of the fluorescent material quality, pure water consumption are 3 times of the fluorescent material quality, disperse 1.5 rev/mins of rotating speeds, jitter time 2 hours;
5) fluorescent material that clears branch sieves through 500 order nylon screens under the flushing of pure water; Wash the fluorescent material that branch clears, the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
The powder slurry (fluorescent material and pure water) intact water sieve carries out fluorescent material and water sepn with centrifuge dewatering; Put into the inherent electricity of fine aluminium plate to the fluorescent material that has dewatered or steam dryer carries out drying, drying temperature is that 120 ℃, time of drying are 10Hr;
The fluorescent material good drying sieves with 500 order nylon screens, obtains FED and uses red luminescence phosphor.
Like Fig. 1, the micro-view of particle shown in Figure 2, the FED of above-mentioned preparation can reach 2～8 μ m with the grain diameter of red luminescence phosphor (yttrium europium oxide terbium), satisfies the requirement of FED with fluorescent material.
Prepared FED is as shown in Figure 3 with the stimulated luminescence spectrogram of red luminescence phosphor (yttrium europium oxide terbium); Can see after being excited; Its luminous intensity is compared with conventional red luminescence phosphor (yttrium europium oxide) luminous intensity, has higher luminosity (having exceeded 10～20%).
Claims (9)
1. a FED uses red luminescence phosphor, it is characterized in that, this fluorescent material is the coactivated fluorescent material of europium and terbium, by quality ratio, and yttrium oxide: europium sesquioxide: terbium sesquioxide=(92～97): (2.5～7.5): (0.001～0.005).
2. FED as claimed in claim 1 uses red luminescence phosphor, it is characterized in that, by quality ratio, yttrium oxide: europium sesquioxide: terbium sesquioxide=(92.55～96.55): (3.45～7.45): (0.002～0.003).
3. a FED is characterized in that with the preparation method of red luminescence phosphor, may further comprise the steps:
1) according to yttrium oxide: europium sesquioxide: terbium sesquioxide=(92～97): (2.5～7.5): the mass ratio of (0.001～0.005); With yttrium oxide, europium sesquioxide, terbium sesquioxide thorough mixing; And then add the bariumchloride of mixing back quality 1.5～3.5% and 0.10～0.15% boric acid thorough mixing, obtain the fluorescence powder;
2) the fluorescence powder is packed in the airtight container, at 1200～1500 ℃ of following heat preservation sintering 4～6h;
3) fluorescent material that burns till is taken out the back and pulverize, wet method is dispersed into slurry, is disperseing to cross simultaneously 100～200 eye mesh screens, and fluorescent material is collected in dehydration then;
4) fluorescent material of collecting that will dewater disperses in dispersion machine, and the fluorescent material water flushing that clears branch is down through 300～500 eye mesh screens, then with fluorescent material with water washing 6～9 times, wash churning time 15～30min, the fluorescent material of dehydration collection at last at every turn;
5) the fluorescent material that has dewatered dry 4～24h under 100～150 ℃; Cross 300～500 eye mesh screens to the good fluorescent material of drying, obtain FED and use red luminescence phosphor.
4. FED as claimed in claim 3 is with the preparation method of red luminescence phosphor; It is characterized in that; The thorough mixing of described yttrium oxide, europium sesquioxide, terbium sesquioxide is that it is processed the heavy altogether article of yttrium europium oxide terbium that granularity is 3.0～5.0 μ m in proportion, and then adds the yttrium europium oxide terbium and sink the bariumchloride of quality 1.5～3.5% and 0.10～0.15% boric acid thorough mixing altogether.
5. FED as claimed in claim 4 is with the preparation method of red luminescence phosphor; It is characterized in that; Being mixed into of fluorescence powder:, in mixer, mix 60～120min afterwards with mistake 100 eye mesh screens behind the heavy altogether article of yttrium europium oxide terbium and bariumchloride, the boric acid mixed grinding.
Like claim 3 or 5 described FED with the preparation method of red luminescence phosphor, it is characterized in that described bariumchloride also carries out following pre-treatment: with bariumchloride at 100～130 ℃ of 3～6h when dry down.
Like claim 3 or 5 described FED with the preparation method of red luminescence phosphor, it is characterized in that, described airtight container be airtight alumina crucible.
8. like claim 3 or 5 described FED preparation method with red luminescence phosphor; It is characterized in that; The described fluorescent material collected of will dewatering disperses in liner is the dispersion machine of ceramic tile, and dispersion condition is 2～3 times of the fluorescent material quality, the dispersion glass sphere of diameter 2.5～5mm, and water consumption is 1～3 times of fluorescent material quality; The dispersion rotating speed is 1.5～4.0r/min, jitter time 1.5～3h.
Like claim 3 or 5 described FED with the preparation method of red luminescence phosphor, it is characterized in that it is to carry out centrifuge dehydration with whizzer that fluorescent material is collected in said dehydration.
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| CN103305223A (en) * | 2012-09-07 | 2013-09-18 | 彩虹集团电子股份有限公司 | Manufacturing method of red fluorescent powder for tri-phosphor energy saving lamp |
| CN103305209A (en) * | 2013-04-13 | 2013-09-18 | 兰州大学 | Fluxing agent for preparing Y2O3:Eu red phosphor |
| CN117143601A (en) * | 2023-08-16 | 2023-12-01 | 东台市天源光电科技有限公司 | Color-adjustable nano rare earth anti-counterfeiting fluorescent powder and preparation method thereof |
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