CN101565613A - Method for producing zinc-manganese silicate green fluorescent powder for PDP - Google Patents
Method for producing zinc-manganese silicate green fluorescent powder for PDP Download PDFInfo
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- CN101565613A CN101565613A CN 200910022775 CN200910022775A CN101565613A CN 101565613 A CN101565613 A CN 101565613A CN 200910022775 CN200910022775 CN 200910022775 CN 200910022775 A CN200910022775 A CN 200910022775A CN 101565613 A CN101565613 A CN 101565613A
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Abstract
The invention relates to a method for producing fluorescent powder, in particular to a method for producing zinc-manganese silicate green fluorescent powder for a PDP. The method comprises the following steps: firstly, weighing ZnO, SiO2, Mn2CO3 and a small amount of fluxing agent according to certain proportion, putting the materials into a mixer, adding alcohol to the materials and then mixing the materials evenly; secondly, drying and screening the mixed material and then filling the mixture into a crucible, burning the mixture in a tunnel furnace in an inert or reducing atmosphere, and cooling the mixture to the room temperature; thirdly, screening the burnt powder agglomates and then putting the same into a dispersion machine to disperse powder, and washing, drying and screening the powder; and finally, refilling the powder subjected to dispersing, washing, drying and screening into the crucible, burning the powder again in the inert or reducing atmosphere, cooling the powder to the room temperature, and screening the powder to obtain the zinc-manganese silicate green fluorescent powder for the PDP. The green fluorescent powder prepared by the method has complete crystal surfaces and mechanisms and good luminescence properties, and improves the defects of large light decay, poor luminescence properties and the like after the screen-loading of the powder.
Description
One, technical field:
The present invention relates to a kind of manufacture method of fluorescent material, particularly a kind of PDP manufacture method of manganese zinc silicate green fluorescent powder.
Two, background technology:
PDP adopts high temperature solid-state synthetic with the manganese zinc silicate green fluorescent powder industrial production usually, and its advantage is that synthesis technique equipment is simple relatively, stable processing technique, and yield is higher.But, powder plane of crystal and structure are destroyed because of high temperature solid phase synthesis production powder aftertreatment intensity is big; Simultaneously, the 147nm ultraviolet ray that discharge generation intensity is very big in the PDP unit, i.e. PDP fluorescent material excitation light source, it is big again to the powder intensity of burning, and these factors make that finally the back brightness decay of powder dress screen is fast.
Three, summary of the invention:
The object of the present invention is to provide a kind of PDP manufacture method with manganese zinc silicate green fluorescent powder, the powder light decay that traditional technology makes is big to solve, the characteristics of luminescence etc. problem.
For achieving the above object, the present invention includes following steps:
Feedstock production
(1) with mol ratio Zn/Si=1.5～1.9, Mn/Si=0.045～0.065, with ZnO, SiO
2, Mn
2CO
3And the fusing assistant thorough mixing, obtain mixture A; Described fusing assistant addition is ZnO, SiO
2, Mn
2CO
30.2～2% of gross weight;
(2) again by mixture A: alcohol: ball is that 1: 2: 1 mass ratio mixes, and obtains mixture B;
(3) mixture B is dropped into the mixer abundant mixing that rolls, will obtain mixture C after reclaiming by alcohol among the mixture B then;
(4) mixture C is also crossed the phosphor raw material that 100 mesh sieves must mix 80～100 ℃ of dry backs;
Once-firing
(5) phosphor raw material was burnt till 3～5 hours under 1050～1350 ℃ of inertia or reducing atmosphere, be cooled to naturally and cross 100 mesh sieves after the room temperature and obtain fluorescent material once-firing product;
The once-firing product are handled
(6) by fluorescent material once-firing product: water: ball is after 1: 2～4: 2～4 mass ratio mixes, to drop into dispersion machine, obtains the powder slurry after Ball milling, after powder slurry washed, dewaters, 100～120 ℃ down dry, dry powder is crossed 160 mesh sieves after being cooled to room temperature, obtain the fluorescent material first product;
Twice firing
(7) the fluorescent material first product being placed temperature in the stove is 200 ℃ electric continuous tunnel furnace, under inertia or reducing atmosphere, with heat-up rate is under the situation of 40～80 ℃/h, begin to heat up from 200 ℃, be warming up to 800～900 ℃ of insulations 0.5～1.5 hour, be 40～80 ℃/h with heat-up rate then, being warming up to 1000～1200 ℃ again burnt till 0.5～2.0 hour, be 40～80 ℃/h with cooling rate again, be cooled to 200 ℃, fluorescent material is taken out from electric continuous tunnel furnace, naturally cooled to room temperature then, sieving obtains the fluorescent material finished product.
Above-mentioned fusing assistant is Li
2CO
3, H
3BO
3, ZnF
2, BaB
4O
7, BaF
2In one or more.
Above-mentioned fusing assistant with ZnO, SiO
2, Mn
2CO
3Cross 100 mesh sieves before mixing.
Inert atmosphere described in above-mentioned steps (5) and the step (7) is N
2Or N
2A kind of among the-Ar, its flow is 2～15m
3/ h;
Reducing atmosphere described in above-mentioned steps (5) and the step (7) is the mixed gas of hydrogen and nitrogen, and the volume ratio of hydrogen and nitrogen is 1: 16～2000.
Reducing atmosphere described in above-mentioned steps (5) and the step (7) is N
2-powdered carbon, powdered carbon cover the powder upper surface fully.
The present invention in manufacturing process by powder being carried out the secondary inertia or the reducing atmosphere reparation is burnt till, perfect powder granule structure and pattern, thus made the PDP green emitting phosphor that the light decay performance is excellent, luminescent properties is good.
Four, embodiment:
Embodiment 1:
Feedstock production
(1) with mol ratio Zn/Si=1.65, Mn/Si=0.045 with ZnO, SiO
2, Mn
2CO
3And the fusing assistant thorough mixing obtains mixture A.Described fusing assistant is Li
2CO
3, Li
2CO
3Addition be ZnO, SiO
2, Mn
2CO
30.2% of gross weight; Li
2CO
3With ZnO, SiO
2, Mn
2CO
3Cross 100 mesh sieves before mixing.
(2) again by mixture A: alcohol: ball is that 1: 2: 1 mass ratio mixes, and obtains mixture B;
(3) mixture B is dropped into mixer and rolled 8 hours, obtain mixture C after then alcohol among the mixture B being reclaimed;
(4) mixture C is also crossed the phosphor raw material that 100 mesh sieves must mix 80 ℃ of dry backs.
Once-firing
(5) phosphor raw material is packed into alumina crucible and be nitrogen at 1150 ℃, inert atmosphere, nitrogen flow is 15m
3The electric continuous tunnel furnace burnt till 5 hours under the situation of/h, was cooled to naturally to cross 100 mesh sieves after the room temperature and obtain fluorescent material once-firing product.
The once-firing product are handled
(6) by fluorescent material once-firing product: water: ball is after 1: 2: 2 mass ratio mixes, to drop into dispersion machine, obtains the powder slurry after Ball milling, the powder slurry is carried out 2 washings, dehydration, then 100 ℃ of dryings 10 hours, dry powder is crossed 160 mesh sieves after being cooled to room temperature, obtain the fluorescent material first product.
Twice firing
(7) the fluorescent material first product being packed into to place temperature in the stove be 200 ℃ electric continuous tunnel furnace to alumina crucible, is N at reducing atmosphere
2-powdered carbon, powdered carbon covers the powder upper surface fully, and heat-up rate is under the situation of 40 ℃/h, begins to heat up from 200 ℃, be warming up to 800 ℃ of insulations 1.0 hours, being 40 ℃/h with heat-up rate then, being warming up to 1050 ℃ again and burning till 0.5 hour, is 40 ℃/h with cooling rate again, be cooled to 200 ℃, fluorescent material is taken out from electric continuous tunnel furnace, naturally cooled to room temperature then, cross 160 mesh sieves and obtain fluorescent material sample 1.
Embodiment 2:
Feedstock production
(1) with mol ratio Zn/Si=1.75, Mn/Si=0.055 with ZnO, SiO
2, Mn
2CO
3And the fusing assistant thorough mixing obtains mixture A.Described fusing assistant is Li
2CO
3And ZnF
2By mass ratio is the mixture of 1: 1 mixed.The addition of solubility promoter is ZnO, SiO
2, Mn
2CO
31.5% of gross weight; Fusing assistant with ZnO, SiO
2, Mn
2CO
3Cross 100 mesh sieves before mixing.
(2) again by mixture A: alcohol: ball is that 1: 2: 1 mass ratio mixes, and obtains mixture B;
(3) mixture B is dropped into mixer and rolled 10 hours, obtain mixture C after then alcohol among the mixture B being reclaimed;
(4) mixture C is also crossed the phosphor raw material that 100 mesh sieves must mix 100 ℃ of dry backs.
Once-firing
(5) phosphor raw material is packed into alumina crucible and be N at 1200 ℃, inert atmosphere
2-Ar, N
2-Ar total flux is 8m
3The electric continuous tunnel furnace burnt till 3 hours under the situation of/h, was cooled to naturally to cross 100 mesh sieves after the room temperature and obtain fluorescent material once-firing product.
The once-firing product are handled
(6) by fluorescent material once-firing product: water: ball is after 1: 2: 3 mass ratio mixes, to drop into dispersion machine, obtains the powder slurry after Ball milling, the powder slurry is carried out 3 washings, dehydration, then 120 ℃ of dryings 12 hours, dry powder is crossed 160 mesh sieves after being cooled to room temperature, obtain the fluorescent material first product.
Twice firing
(7) the fluorescent material first product being packed into to place temperature in the stove be 200 ℃ electric continuous tunnel furnace to alumina crucible, is H at reducing atmosphere
2And N
2Mixed gas, the volume ratio of hydrogen and nitrogen is 1: 2000, and heat-up rate is under the situation of 70 ℃/h, begins to heat up from 200 ℃, be warming up to 850 ℃ of insulations 0.5 hour, being 70 ℃/h with heat-up rate then, being warming up to 1150 ℃ again and burning till 1 hour, is 70 ℃/h with cooling rate again, be cooled to 200 ℃, fluorescent material is taken out from electric continuous tunnel furnace, naturally cooled to room temperature then, cross 160 mesh sieves and obtain fluorescent material sample 2.
Embodiment 3:
(1) with mol ratio Zn/Si=1.50, Mn/Si=0.050 with ZnO, SiO
2, Mn
2CO
3And the fusing assistant thorough mixing obtains mixture A.Described fusing assistant is BaF
2, solubility promoter BaF
2Addition be ZnO, SiO
2, Mn
2CO
30.7% of gross weight; BaF
2With ZnO, SiO
2, Mn
2CO
3Cross 100 mesh sieves before mixing.
(2) again by mixture A: alcohol: ball is that 1: 2: 1 mass ratio mixes, and obtains mixture B;
(3) mixture B is dropped into mixer and rolled 12 hours, obtain mixture C after then alcohol among the mixture B being reclaimed;
(4) mixture C is also crossed the phosphor raw material that 100 mesh sieves must mix 100 ℃ of dry backs.
Once-firing
(5) phosphor raw material is packed into alumina crucible is H at 1350 ℃, reducing atmosphere
2And N
2Mixed gas, the volume ratio of hydrogen and nitrogen is that 1: 500 electric continuous tunnel furnace under the situation burnt till 5 hours, is cooled to naturally to cross 100 mesh sieves after the room temperature and obtain fluorescent material once-firing product.
The once-firing product are handled
(6) by fluorescent material once-firing product: water: ball is after 1: 3: 3 mass ratio mixes, to drop into dispersion machine, obtains the powder slurry after Ball milling, the powder slurry is carried out 4 washings, dehydration, then 110 ℃ of dryings 10 hours, dry powder is crossed 160 mesh sieves after being cooled to room temperature, obtain the fluorescent material first product.
Twice firing
(7) the fluorescent material first product being packed into to place temperature in the stove be 200 ℃ electric continuous tunnel furnace to alumina crucible, is N at reducing atmosphere
2-powdered carbon, powdered carbon covers the powder upper surface fully, and heat-up rate is under the situation of 60 ℃/h, begins to heat up from 200 ℃, be warming up to 800 ℃ of insulations 1 hour, being 60 ℃/h with heat-up rate then, being warming up to 1200 ℃ again and burning till 1.5 hours, is 60 ℃/h with cooling rate again, be cooled to 200 ℃, fluorescent material is taken out from electric continuous tunnel furnace, naturally cooled to room temperature then, cross 160 mesh sieves and obtain fluorescent material sample 3.
Embodiment 4:
(1) with mol ratio Zn/Si=1.9, Mn/Si=0.065 with ZnO, SiO
2, Mn
2CO
3And the fusing assistant thorough mixing obtains mixture A.Described fusing assistant is Li
2CO
3And H
3BO
31: 2 in molar ratio blended mixture.The addition of solubility promoter is ZnO, SiO
2, Mn
2CO
31.2% of gross weight; Solubility promoter with ZnO, SiO
2, Mn
2CO
3Cross 100 mesh sieves before mixing.
(2) again by mixture A: alcohol: ball is that 1: 2: 1 mass ratio mixes, and obtains mixture B;
(3) mixture B is dropped into mixer and rolled 8 hours, obtain mixture C after then alcohol among the mixture B being reclaimed;
(4) mixture C is also crossed the phosphor raw material that 100 mesh sieves must mix 90 ℃ of dry backs.
Once-firing
(5) phosphor raw material is packed into alumina crucible and be N at 1050 ℃, reducing atmosphere
2The electric continuous tunnel furnace that-powdered carbon, powdered carbon cover under the situation of powder upper surface fully burnt till 4 hours, was cooled to naturally to cross 100 mesh sieves after the room temperature and obtain fluorescent material once-firing product.
The once-firing product are handled
(6) by fluorescent material once-firing product: water: ball is after 1: 4: 2 mass ratio mixes, to drop into dispersion machine, obtains the powder slurry after Ball milling, the powder slurry is carried out 4 washings, dehydration, then 120 ℃ of dryings 14 hours, dry powder is crossed 160 mesh sieves after being cooled to room temperature, promptly get the fluorescent material first product.
Twice firing
(7) the fluorescent material first product being packed into to place temperature in the stove be 200 ℃ electric continuous tunnel furnace to alumina crucible, is N at inert atmosphere
2-Ar, N
2-Ar total flux is 2m
3/ h,, heat-up rate is under the situation of 80 ℃/h, begins to heat up from 200 ℃, be warming up to 900 ℃ of insulations 1.5 hours, being 80 ℃/h with heat-up rate then, being warming up to 1000 ℃ again and burning till 1.0 hours, is 80 ℃/h with cooling rate again, be cooled to 200 ℃, fluorescent material is taken out from electric continuous tunnel furnace, naturally cooled to room temperature then, cross 160 mesh sieves and obtain fluorescent material sample 4.
By contrast green emitting phosphor sample (sample 1～4) that above-mentioned 4 embodiment draw and in the market PDP obtain table 1 with the performance perameter between the manganese zinc silicate green fluorescent powder (with reference to sample):
| Lot number | Chromaticity coordinates (x) | Chromaticity coordinates (y) | Brightness (%) | Light decay (%) |
| With reference to sample | 0.242 | 0.701 | 94 | 22 |
| Sample 1 | 0.239 | 0.702 | 102 | 12 |
| Sample 2 | 0.242 | 0.702 | 100 | 9 |
| Sample 3 | 0.243 | 0.702 | 99 | 10 |
| Sample 4 | 0.242 | 0.702 | 99 | 8 |
From last table we as can be seen, the brightness value of sample 1～4 is apparently higher than the brightness value of reference sample; The light decay value is less than the light decay value of reference sample, and novel Mingguang City performance that declines is excellent more more for the light decay value, and light decay performance that can interpret sample 1～4 is significantly better than the light decay performance of reference sample.
Claims (6)
1. the manufacture method of a PDP usefulness manganese zinc silicate green fluorescent powder is characterized in that: may further comprise the steps
Feedstock production
(1) with mol ratio Zn/Si=1.5～1.9, Mn/Si=0.045～0.065, with ZnO, SiO
2, Mn
2CO
3And the fusing assistant thorough mixing, obtain mixture A; Described fusing assistant addition is ZnO, SiO
2, Mn
2CO
30.2～2% of gross weight;
(2) again by mixture A: alcohol: ball is that 1: 2: 1 mass ratio mixes, and obtains mixture B;
(3) mixture B is dropped into the mixer abundant mixing that rolls, will obtain mixture C after reclaiming by alcohol among the mixture B then;
(4) mixture C is also crossed the phosphor raw material that 100 mesh sieves must mix 80～100 ℃ of dry backs;
Once-firing
(5) phosphor raw material was burnt till 3～5 hours under 1050～1350 ℃ of inertia or reducing atmosphere, be cooled to naturally and cross 100 mesh sieves after the room temperature and obtain fluorescent material once-firing product;
The once-firing product are handled
(6) by fluorescent material once-firing product: water: ball is after 1: 2～4: 2～4 mass ratio mixes, to drop into dispersion machine, obtains the powder slurry after Ball milling, after powder slurry washed, dewaters, 100～120 ℃ down dry, dry powder is crossed 160 mesh sieves after being cooled to room temperature, obtain the fluorescent material first product;
Twice firing
(7) the fluorescent material first product being placed temperature in the stove is 200 ℃ electric continuous tunnel furnace, under inertia or reducing atmosphere, with heat-up rate is under the situation of 40～80 ℃/h, begin to heat up from 200 ℃, be warming up to 800～900 ℃ of insulations 0.5～1.5 hour, be 40～80 ℃/h with heat-up rate then, being warming up to 1000～1200 ℃ again burnt till 0.5～2.0 hour, be 40～80 ℃/h with cooling rate again, be cooled to 200 ℃, fluorescent material is taken out from electric continuous tunnel furnace, naturally cooled to room temperature then, sieving obtains the fluorescent material finished product.
2, a kind of PDP according to claim 1 manufacture method of manganese zinc silicate green fluorescent powder, it is characterized in that: described fusing assistant is Li
2CO
3, H
3BO
3, ZnF
2, BaB
4O
7, BaF
2In one or more.
3, a kind of PDP according to claim 1 and 2 is characterized in that with the manufacture method of manganese zinc silicate green fluorescent powder: described fusing assistant with ZnO, SiO
2, Mn
2CO
3Cross 100 mesh sieves before mixing.
4, a kind of PDP according to claim 1 manufacture method of manganese zinc silicate green fluorescent powder, it is characterized in that: the inert atmosphere described in step (5) and the step (7) is N
2Or N
2A kind of among the-Ar, its flow is 2～15m
3/ h;
5, according to the manufacture method of claims 1 described a kind of PDP with manganese zinc silicate green fluorescent powder, it is characterized in that: the reducing atmosphere described in step (5) and the step (7) is the mixed gas of hydrogen and nitrogen, and the volume ratio of hydrogen and nitrogen is 1: 16～2000.
6, according to the manufacture method of claims 1 described a kind of PDP with manganese zinc silicate green fluorescent powder, it is characterized in that: the reducing atmosphere described in step (5) and the step (7) is N
2-powdered carbon, powdered carbon cover the powder upper surface fully.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910022775 CN101565613A (en) | 2009-06-01 | 2009-06-01 | Method for producing zinc-manganese silicate green fluorescent powder for PDP |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910022775 CN101565613A (en) | 2009-06-01 | 2009-06-01 | Method for producing zinc-manganese silicate green fluorescent powder for PDP |
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| Publication Number | Publication Date |
|---|---|
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|---|---|---|---|
| CN 200910022775 Pending CN101565613A (en) | 2009-06-01 | 2009-06-01 | Method for producing zinc-manganese silicate green fluorescent powder for PDP |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676152A (en) * | 2012-05-09 | 2012-09-19 | 苏州英特华照明有限公司 | Flux for preparing green fluorescent powder for light emitting diode (LED) |
| CN103131408A (en) * | 2012-10-16 | 2013-06-05 | 彩虹集团公司 | High-temperature post-processing method of silicate green fluorescent powder |
| CN103773363A (en) * | 2013-12-17 | 2014-05-07 | 中国计量学院 | Green manganese-activated zinc silicate fluorescent powder and preparation method thereof |
-
2009
- 2009-06-01 CN CN 200910022775 patent/CN101565613A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676152A (en) * | 2012-05-09 | 2012-09-19 | 苏州英特华照明有限公司 | Flux for preparing green fluorescent powder for light emitting diode (LED) |
| CN102676152B (en) * | 2012-05-09 | 2014-12-24 | 英特美光电（苏州）有限公司 | Flux for preparing green fluorescent powder for light emitting diode (LED) |
| CN103131408A (en) * | 2012-10-16 | 2013-06-05 | 彩虹集团公司 | High-temperature post-processing method of silicate green fluorescent powder |
| CN103131408B (en) * | 2012-10-16 | 2014-12-10 | 彩虹集团公司 | High-temperature post-processing method of silicate green fluorescent powder |
| CN103773363A (en) * | 2013-12-17 | 2014-05-07 | 中国计量学院 | Green manganese-activated zinc silicate fluorescent powder and preparation method thereof |
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Application publication date: 20091028 |