CN101597491A - A kind of manufacture method of green emitting phosphor powder for field emission display - Google Patents
A kind of manufacture method of green emitting phosphor powder for field emission display Download PDFInfo
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- CN101597491A CN101597491A CNA2009100231433A CN200910023143A CN101597491A CN 101597491 A CN101597491 A CN 101597491A CN A2009100231433 A CNA2009100231433 A CN A2009100231433A CN 200910023143 A CN200910023143 A CN 200910023143A CN 101597491 A CN101597491 A CN 101597491A
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Abstract
The invention belongs to fluorescent material manufacturing technology field, be particularly related to a kind of manufacture method of green light-emitting fluorescent powder, comprise the steps: 1) making of 2500ppm concentration copper powder: 2) batching: with zinc sulphide, copper powder, activator, solubility promoter mixed grinding, sieve, in mixer, mix; 3) charging: the sulphur of in quartz crucible, packing into, gac covers quartz crucible completely with quartz cover; 4) burn till; 5) select powder: get rid of not luminous or luminous unusual powder and impurity; 6) water sieve: fluorescent material sieves in the flushing of pure water; 7) wash 8) the top coat processing: 9) anhydrate: 10) dry 11) sieve powder obtains the FED green emitting phosphor.FED of the present invention has the brightness height with green light-emitting fluorescent powder, narrow particle size distribution, and fluorescent powder grain is even, has promoted the yield of fluorescent material; Technology is simple, and process cycle is short, makes safety.
Description
Affiliated field:
The invention belongs to fluorescent material manufacturing technology field, particularly a kind of manufacture method of green light-emitting fluorescent powder.
Prior art
At present, field-emitter display FED is mainly strontium thiogallate europium green emitting phosphor with green light-emitting fluorescent powder and ZnS is the matrix green emitting phosphor, strontium thiogallate europium green emitting phosphor is europkium-activated, its manufacture method is to burn till for twice, burn till for oxidation for the first time, burn till for reduction for the second time, its reducing atmosphere is that hydrogen sulfide and nitrogen add hydrogen, there is shortcoming in the manufacture method of this powder: complex process, process cycle is long, the quality of powder especially brightness and colourity consistence is poor, owing to use hydrogen sulfide and hydrogen, there is unsafe factor in manufacturing processed in addition; Though and that normally used ZnS is a matrix green emitting phosphor process cycle is shorter than strontium thiogallate europium green emitting phosphor, does not also have hydrogen sulfide and hydrogen atmosphere, has the wide shortcoming of fluorescent material low lightness and MODEL OF THE PHOSPHOR PARTICLE SIZE DISTRIBUTION.
Summary of the invention:
The complex process of firing with green light-emitting fluorescent powder at field-emitter display FED in the prior art, process cycle are long, the technical problem of the quality conformance difference of powder, the present invention proposes the manufacture method of a kind of FED with green light-emitting fluorescent powder, comprises the steps:
1, the making of 2500ppm concentration copper powder: with the zinc sulphide of electronics weigh scale amount 10kg, the measured zinc sulphide of scale is placed on paving in the fine aluminium plate of pure water wash clean and zinc sulphide, activator cupric nitrate with electronics weigh scale amount 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the 1000ml glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens afterwards, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine afterwards and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, promptly made 2500ppm concentration copper powder.
2, the batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 3.2～10%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.02715～0.04265%, after the solubility promoter barium iodide amount of quoting is 0.10～0.18% mixed grinding of zinc sulphide quality, add sulphur, the sulphur amount of quoting is 2.5～12% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 20～200g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixes 30～120min, the fluorescence powder that obtains mixing;
3, charging: the above-mentioned fluorescence powder that the prepares 1.0～2.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 20～30% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 20～30% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4, burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 950～990 ℃ of firing temperatures; Firing time 2～4Hr;
5, select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6, water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7, washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 10～15min at every turn;
8, top coat is handled: the pure water consumption is 2～4 times of fluorescent material quality, fluorescent material powder slurry (fluorescent material powder slurry is exactly fluorescent material and pure water) is stirred 10～15min, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 10～15min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 10～15min;
9, anhydrate: the fluorescent material centrifugal force that top coat is handled well is that the water extracter or the vacuum filtration of principle anhydrates;
10, drying: the fluorescent material that anhydrates is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ± 10 ℃, time of drying are 4～8Hr;
11, sieve powder: the fluorescent material good drying sieves with 300～500 order nylon screens.
FED of the present invention has with green light-emitting fluorescent powder: 1, brightness height, and narrow particle size distribution, fluorescent powder grain is even, has promoted the yield of fluorescent material; 2, technology is simple, and process cycle is short, makes safety.
Embodiment
Use in the step 2 among the present invention activator γ-Al
2O
3Content 〉=99%, specific surface area be 85～115m
2/ g, pH value are 4.5～5.5 (4% aqueous solution tests), Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%;
Content 〉=99%, water-insoluble≤0.01%, muriate and the bromide of the solubility promoter barium iodide that uses in the step 2 among the present invention are (with Cl
-Meter)≤0.05%, iodine and iodate are (with IO
3 -Meter)≤0.01%, Fe≤10ppm, Pb≤10ppm, basic metal and calcium (in vitriol)≤0.25%;
Content＞99.5%, Fe content≤0.3ppm, Pb content≤0.5ppm, the Ni content≤0.5ppm of the sulphur that uses in step 2 neutralization procedure 3 among the present invention;
The gac that uses in the step 2 among the present invention is the coconut husk charcoal;
The concentration of the 3.05 modulus potassium silicate solutions that use in the step 8 among the present invention is 25 ± 0.2%, and its 3.05 modulus is SiO
2And K
2The mol ratio of O.
Embodiment 1
1) making of 2500ppm concentration copper powder: the zinc sulphide of 10kg is placed in the fine aluminium plate with the pure water wash clean paves, the activator cupric nitrate of weighing 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, obtained the copper powder of 2500ppm concentration.
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 3.2%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.02715%, the solubility promoter barium iodide amount of quoting is 0.10% of zinc sulphide quality, behind the mixed grinding, add sulphur, the sulphur amount of quoting is 2.5% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 20g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixing 30min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 1.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 20% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 20% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of fluorescence powder of 1.5kg in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 950 ℃ of firing temperatures; Firing time 2Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 10min at every turn;
8) top coat is handled: the pure water consumption is 2 times of fluorescent material quality, the fluorescent material powder slurry of fluorescent material and pure water formation is stirred, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 10min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 10min;
9) anhydrate: the fluorescent material that top coat is handled well anhydrates with centrifuge or vacuum filtration;
10) drying: the fluorescent material after anhydrating is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains the FED green emitting phosphor.
Embodiment 2
1) making of 2500ppm concentration copper powder: with the zinc sulphide of electronics weigh scale amount 10kg, the measured zinc sulphide of scale is placed on paving in the fine aluminium plate of pure water wash clean and zinc sulphide, activator cupric nitrate with electronics weigh scale amount 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the 1000ml glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens afterwards, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine afterwards and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, promptly made 2500ppm concentration copper powder.
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 4%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.04265%, the solubility promoter barium iodide amount of quoting is 0.125% of zinc sulphide quality, behind the mixed grinding, add sulphur, the sulphur amount of quoting is 2.5% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 40g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixing 120min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 1.5kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 30% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 30% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescent material burning in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 980 ℃ of firing temperatures; Firing time 4Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
8) top coat is handled: the pure water consumption is 4 times of fluorescent material quality, fluorescent material powder slurry (fluorescent material powder slurry is exactly fluorescent material and pure water) is stirred 10min, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 10min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 10min;
9) anhydrate: the fluorescent material centrifugal force that top coat is handled well is that the water extracter or the vacuum filtration of principle anhydrates;
10) drying: the fluorescent material that anhydrates is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains the FED green emitting phosphor.
Embodiment 3
1) making of 2500ppm concentration copper powder: with the zinc sulphide of electronics weigh scale amount 10kg, the measured zinc sulphide of scale is placed on paving in the fine aluminium plate of pure water wash clean and zinc sulphide, activator cupric nitrate with electronics weigh scale amount 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the 1000ml glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens afterwards, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine afterwards and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, promptly made 2500ppm concentration copper powder.
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 10%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.0349%, the solubility promoter barium iodide amount of quoting is 0.18% of zinc sulphide quality, behind the mixed grinding, add sulphur, the sulphur amount of quoting is 8% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 200g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixing 60min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 2.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 25% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 25% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 990 ℃ of firing temperatures; Firing time 2.5Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 12min at every turn;
8) top coat is handled: the pure water consumption is 3 times of fluorescent material quality, fluorescent material powder slurry (fluorescent material powder slurry is exactly fluorescent material and pure water) is stirred 15min, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 15min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 15min;
9) anhydrate: the fluorescent material centrifugal force that top coat is handled well is that the water extracter or the vacuum filtration of principle anhydrates;
10) drying: the fluorescent material that anhydrates is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 500 order nylon screens, obtains the FED green emitting phosphor.
Embodiment 4
1) making of 2500ppm concentration copper powder: the zinc sulphide of 10kg is placed in the fine aluminium plate with the pure water wash clean paves, the activator cupric nitrate of weighing 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, obtained the copper powder of 2500ppm concentration.
2) batching: 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 10%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.04265%, the solubility promoter barium iodide amount of quoting is that 0.18% and the sulphur amount of quoting of zinc sulphide quality is 12% of zinc sulphide quality, good with electronics weigh scale amount above-mentioned materials by processing requirement, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 200g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur is blended in and mixes 120min in the mixer;
3) charging: the above-mentioned fluorescence powder that the prepares 2.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 30% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 30% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 990 ℃ of firing temperatures; Firing time 4Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
8) top coat is handled: the pure water consumption is 4 times of fluorescent material quality, the fluorescent material powder slurry of fluorescent material and pure water formation is stirred, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 15min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 15min;
9) anhydrate: the fluorescent material that top coat is handled well anhydrates with centrifuge or vacuum filtration;
10) drying: the fluorescent material after anhydrating is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains the FED green emitting phosphor.
Claims (9)
1. the manufacture method of a green emitting phosphor powder for field emission display is characterized in that, comprises the steps:
1) making of 2500ppm concentration copper powder: the zinc sulphide of 10kg is placed in the fine aluminium plate with the pure water wash clean paves, the activator cupric nitrate of weighing 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, obtained the copper powder of 2500ppm concentration;
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 3.2～10%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.02715～0.04265%, after the solubility promoter barium iodide amount of quoting is 0.10～0.18% mixed grinding of zinc sulphide quality, add sulphur, the sulphur amount of quoting is 2.5～12% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 20～200g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixes 30～120min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 1.0～2.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 20～30% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 20～30% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 950～990 ℃ of firing temperatures; Firing time 2～4Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 10～15min at every turn;
8) top coat is handled: with the pure water mixing and stirring of fluorescent material and 2-4 times of fluorescent material quality, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 10～15min, the solution of zinc sulfate that adds 0.7 mole again, its consumption is that every kilogram of fluorescent material uses 60ml, stirs 10～15min;
9) anhydrate: the fluorescent material that top coat is handled well anhydrates with centrifuge or vacuum filtration;
10) drying: the fluorescent material after anhydrating is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains green emitting phosphor powder for field emission display.
2. the manufacture method of green emitting phosphor powder for field emission display according to claim 1 is characterized in that, comprises the steps:
1) making of 2500ppm concentration copper powder: the zinc sulphide of 10kg is placed in the fine aluminium plate with the pure water wash clean paves, the activator cupric nitrate of weighing 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, obtained the copper powder of 2500ppm concentration;
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 3.2%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.02715%, the solubility promoter barium iodide amount of quoting is 0.10% of zinc sulphide quality, behind the mixed grinding, add sulphur, the sulphur amount of quoting is 2.5% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 20g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixing 30min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 1.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 20% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 20% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 950 ℃ of firing temperatures; Firing time 2Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 10min at every turn;
8) top coat is handled: the pure water consumption is 2 times of fluorescent material quality, the fluorescent material powder slurry of fluorescent material and pure water formation is stirred, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 10min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 10min;
9) anhydrate: the fluorescent material that top coat is handled well anhydrates with centrifuge or vacuum filtration;
10) drying: the fluorescent material after anhydrating is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains green emitting phosphor powder for field emission display.
3. the manufacture method of green emitting phosphor powder for field emission display according to claim 1 is characterized in that, comprises the steps:
1) making of 2500ppm concentration copper powder: the zinc sulphide of 10kg is placed in the fine aluminium plate with the pure water wash clean paves, the activator cupric nitrate of weighing 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, obtained the copper powder of 2500ppm concentration;
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 4%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.04265%, the solubility promoter barium iodide amount of quoting is 0.125% of zinc sulphide quality, behind the mixed grinding, add sulphur, the sulphur amount of quoting is 2.5% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 40g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixing 120min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 1.5kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 30% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 30% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 980 ℃ of firing temperatures; Firing time 4Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 15min at every turn;
8) top coat is handled: the pure water consumption is 4 times of fluorescent material quality, the fluorescent material powder slurry of fluorescent material and pure water formation is stirred, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 10min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 10min;
9) anhydrate: the fluorescent material that top coat is handled well anhydrates with centrifuge or vacuum filtration;
10) drying: the fluorescent material after anhydrating is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains green emitting phosphor powder for field emission display.
4. the manufacture method of green emitting phosphor powder for field emission display according to claim 1 is characterized in that, comprises the steps:
1) making of 2500ppm concentration copper powder: the zinc sulphide of 10kg is placed in the fine aluminium plate with the pure water wash clean paves, the activator cupric nitrate of weighing 25g, the measured cupric nitrate of scale is dissolved fully with pure water in the glass beaker with the pure water wash clean, filter copper nitrate solution with 150 order nylon screens, pour in the zinc sulphide in the fine aluminium plate filtering good copper nitrate solution, then beaker is washed 3 times with pure water, wash 3 times pure water and will all pour in the interior zinc sulphide of fine aluminium plate, with pure water zinc sulphide in the fine aluminium plate and copper nitrate solution are mixed fully again; Put into drying machine and carry out drying, 140 ℃ of drying temperatures, time of drying, 14Hr sieved with 130 order nylon screens at last, obtained the copper powder of 2500ppm concentration;
2) batching: with 10kg substrate material zinc sulphide, the 2500ppm concentration copper powder amount of quoting be the zinc sulphide quality 10%, activator γ-Al
2O
3The amount of quoting be the zinc sulphide quality 0.0349%, the solubility promoter barium iodide amount of quoting is 0.18% of zinc sulphide quality, behind the mixed grinding, add sulphur, the sulphur amount of quoting is 8% of a zinc sulphide quality, wherein the solubility promoter barium iodide must and the measured 10kg substrate material of above-mentioned scale zinc sulphide in 200g zinc sulphide mixed grinding, sieve through 130 order nylon screens, afterwards in mixer with remaining substrate material zinc sulphide, activator γ-Al
2O
3And sulphur mixing 60min, the fluorescence powder that obtains mixing;
3) charging: the above-mentioned fluorescence powder that the prepares 2.0kg that in quartz crucible, packs into, the sulphur of in quartz boat, packing into earlier, its amount of quoting is 25% of a quartz crucible dress fluorescence powder quality, reinstall gac, its amount of quoting is 25% of a quartz crucible dress fluorescence powder quality, and makes gac be covered in sulphur fully, afterwards quartz boat is placed on the surface of the fluorescence powder in the above-mentioned quartz crucible, with quartz cover quartz crucible is covered completely, the slit can not be arranged;
4) burn till: in the electric stove in continuous self acting tunnel of nitrogen protection is arranged, burn till 990 ℃ of firing temperatures; Firing time 2.5Hr;
5) select powder: burned fluorescent material is got rid of not luminous or luminous unusual powder and impurity under ultraviolet lamp;
6) water sieve: the fluorescent material of choosing is sieved through 150 order nylon screens under the flushing of pure water;
7) washing: the fluorescent material that water sieve is good is washed, and the pure water consumption is 10 times of fluorescent material quality, and washing times is 6 times, washes churning time 12min at every turn;
8) top coat is handled: the pure water consumption is 3 times of fluorescent material quality, the fluorescent material powder slurry of fluorescent material and pure water formation is stirred, the potassium silicate solution that adds 3.05 moduluses, its consumption is that every kilogram of fluorescent material uses 10ml, stir 15min, the solution of zinc sulfate that adds 0.7 mole, its consumption are that every kilogram of fluorescent material uses 60ml, stir 15min;
9) anhydrate: the fluorescent material that top coat is handled well anhydrates with centrifuge or vacuum filtration;
10) drying: the fluorescent material after anhydrating is put into the inherent steam dryer of fine aluminium plate carry out drying, drying temperature is that 120 ℃, time of drying are 4Hr;
11) sieve powder: the fluorescent material good drying sieves with 300 order nylon screens, obtains green emitting phosphor powder for field emission display.
5. the manufacture method of FED green emitting phosphor according to claim 1 is characterized in that: the activator γ-Al described step 2)
2O
3Content 〉=99%, specific surface area is 85～115m
2/ g, pH value is 4.5～5.5 when 4% aqueous solution test, Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%.
6. the manufacture method of FED green emitting phosphor according to claim 1 is characterized in that: content 〉=99% of the solubility promoter barium iodide described step 2), water insoluble matter content≤0.01% is with Cl
-Timing, muriate and bromide content≤0.05% are with IO
3 -Timing, iodine and iodate content≤0.01%, Fe content≤10ppm, Pb content≤10ppm, with vitriol timing basic metal and calcium contents≤0.25%.
7. the manufacture method of FED green emitting phosphor according to claim 1 is characterized in that: described step 2) with step 3) in content＞99.5% of sulphur, Fe content≤0.3ppm, Pb content≤0.5ppm, Ni content≤0.5ppm.
8. the manufacture method of FED green emitting phosphor according to claim 1 is characterized in that: the gac in the described step 3) is the coconut husk charcoal.
9. the manufacture method of FED green emitting phosphor according to claim 1 is characterized in that: the concentration of 3.05 modulus potassium silicate solutions in the described step 8) is 25 ± 0.2%, and its 3.05 modulus is SiO
2And K
2The mol ratio of O.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992793A (en) * | 2014-05-04 | 2014-08-20 | 徐州工程学院 | Preparation method for high-chroma green phosphor |
| CN104194779A (en) * | 2014-09-02 | 2014-12-10 | 绍兴市越城精佳诚电子材料厂 | Method for preparing green fluorescent powder for VFD (Vacuum Fluorescent Display) |
| CN105829495A (en) * | 2013-12-19 | 2016-08-03 | 联邦印制有限公司 | Zinc Sulphide Phosphor Having Photo-And Electroluminescent Properties, Process For Producing Same, Security Document, Security Feature And Method For Detecting Same |
-
2009
- 2009-06-30 CN CNA2009100231433A patent/CN101597491A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 新梅等: "水热法合成高发光强度ZnS:Cu，Al纳米荧光粉研究", 《功能材料》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105829495A (en) * | 2013-12-19 | 2016-08-03 | 联邦印制有限公司 | Zinc Sulphide Phosphor Having Photo-And Electroluminescent Properties, Process For Producing Same, Security Document, Security Feature And Method For Detecting Same |
| CN105829495B (en) * | 2013-12-19 | 2019-04-23 | 联邦印制有限公司 | Zinc sulphide luminescent material and its manufacturing method and secure file, safety label and its detection method with luminescence generated by light and electroluminescence characters |
| CN103992793A (en) * | 2014-05-04 | 2014-08-20 | 徐州工程学院 | Preparation method for high-chroma green phosphor |
| CN104194779A (en) * | 2014-09-02 | 2014-12-10 | 绍兴市越城精佳诚电子材料厂 | Method for preparing green fluorescent powder for VFD (Vacuum Fluorescent Display) |
| CN104194779B (en) * | 2014-09-02 | 2016-05-04 | 绍兴市越城精佳诚电子材料厂 | The manufacture method of green emitting phosphor for a kind of vacuum fluorescent display |
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