CN101591532B - Method for preparing blue luminescent phosphor for FED - Google Patents
Method for preparing blue luminescent phosphor for FED Download PDFInfo
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- CN101591532B CN101591532B CN 200910022660 CN200910022660A CN101591532B CN 101591532 B CN101591532 B CN 101591532B CN 200910022660 CN200910022660 CN 200910022660 CN 200910022660 A CN200910022660 A CN 200910022660A CN 101591532 B CN101591532 B CN 101591532B
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- fluorescent material
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- fed
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Abstract
The invention discloses a method for preparing blue luminescent phosphor for FED. The method comprises the following steps: (1) preparing 1,000 ppm silver powder; (2) preparing compositions for the luminescent phosphor; (3) loading and sintering the luminescent phosphor; (4) pretreating the luminescent phosphor; (5) treating surface coating; and (6) preparing the blue luminescent phosphor which is obtained through dehydrating, drying and screening treated luminescent powder paste. The method overcomes the defects of low luminescent efficiency and wide grain fineness distribution through adopting new materials for activating agent and fluxing agent and a method for treating the surface coating.
Description
Technical field:
The invention belongs to the fluorescent material field, relate to the manufacture method that a kind of FED uses blue luminescent phosphor.
Background technology:
At present, FED is mainly ZnS:AgAl with blue luminescent phosphor, and its manufacture method is that substrate material zinc sulphide and activator Silver Nitrate, aluminum nitrate and solubility promoter (fusing point is lower than the basic metal of firing temperature, the muriate of III main group metal), sulphur mix under reducing atmosphere through the high temperature solid state reaction generation.The FED blue colour fluorescent powder of this method manufacturing exists luminous efficiency to hang down and the wide shortcoming of size-grade distribution.
Summary of the invention:
The object of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of FED manufacture method with blue luminescent phosphor is provided, the method is according to following steps:
(1) preparation 1000ppm concentration silver powder: 10kg zinc sulphide is paved in the fine aluminium plate; The 10g Silver Nitrate is dissolved in behind the 1000ml glass beaker to filter with 150 eye mesh screens with pure water fully obtains Silver Nitrate filtrate; Add Silver Nitrate filtrate and pure water in the zinc sulphide and be uniformly mixed into mixture, the ratio of zinc sulphide and pure water is 10 in the mixture: 8-12, the effect of pure water is to mix wetting zinc sulphide, as long as zinc sulphide can be mixed, pure water plays the mixing wetting action, its consumption does not affect final effect, and the ratio of preferably getting zinc sulphide and pure water is 10: 8-12; Mixture is carried out sieving with 150 eye mesh screens after the drying, obtain 1000ppm concentration silver powder, wherein 130 ℃ of drying temperatures, 10-14 hour time of drying;
(2) fluorescent material batching: zinc sulphide, 1000ppm concentration silver powder, γ-Al
2O
3, barium iodide and sulphur is 100 according to mass percent: the ratio mixed grinding phosphor mixture of 20-60: 0.02715-0.0565: 0.10-0.20: 2.5-12, phosphor mixture mix 30-120min and obtain the fluorescent material batching in mixer after 100 eye mesh screens sieve;
(3) fluorescent material charging sintering: with the 1.0-2.0kg fluorescent material batching quartz crucible of packing into; The sulphur of packing in quartz boat bottom, sulfur consumption is the 20-30% of fluorescent material batching quality in the quartz crucible, the tight gac that covers on sulphur, activated carbon dosage is the 20-30% of fluorescent material batching quality in the quartz crucible; Then quartz boat is placed on the surface of fluorescent material batching, covers tightly quartz crucible; The quartz crucible that covers tightly sintering in the electric stove of nitrogen protection is obtained pure phosphor, and sintering temperature is that 950～980 ℃, sintering time are 2-4 hour, and adopting agglomerating plant is to burn till in the electric stove in continuous self acting tunnel;
(4) fluorescent material pre-treatment: get rid of under ultraviolet lamp that not luminous or luminous unusual powder obtains qualified pure phosphor in the pure phosphor; Qualified pure phosphor descended 150 eye mesh screen after washings to obtain phosphor slurry in the flushing of pure water; The pure water consumption is 10 times of fluorescent material quality in the described washing, and washing times is 6 times, washes churning time 10-15min at every turn;
(5) top coat is processed: after phosphor slurry is stirred 10-15min, in phosphor slurry, be the potassium silicate solution of 24.8-25.2% according to adding the 10ml concentration of volume percent in every kilogram of fluorescent material, and SiO in the potassium silicate solution
2And K
2The mol ratio of O is 3.05; And then stirring the solution of zinc sulfate that adds 0.7 mole behind the 10-15min, the solution of zinc sulfate consumption is that every kilogram of fluorescent material uses 60ml, last restir 10-15min; Phosphor slurry after obtaining processing;
(6) preparation blue luminescent phosphor: the phosphor slurry after will processing anhydrates, drying, sieve, and obtains blue luminescent phosphor; The drying temperature of described drying is that 110-130 ℃, time of drying are 4-8 hour; Described sieving was the 300-500 eye mesh screen.
Described γ-Al
2O
3Purity 〉=99%, specific surface area is 85～115m
2/ g, pH value are 4.5～5.5 (4% aqueous solution tests), γ-Al
2O
3Middle Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%;
The purity of described barium iodide 〉=99%, the water-insoluble in the barium iodide≤0.01%, muriate and bromide 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%.
The purity of described sulphur＞99.5%, Fe content≤0.3ppm, Pb content≤0.5ppm, Ni content≤0.5ppm in the sulphur.
Described gac is the coconut husk charcoal.
Anhydrating in the described step (6) is to adopt water extracter or vacuum filtration to anhydrate.
Described screen cloth is nylon screen.
The present invention hangs down and the wide shortcoming of size-grade distribution by adopting new activator and flux material and surface coating layer treatment method to solve above-mentioned luminous efficiency.
Embodiment:
The below does the present invention and describes in further detail:
Implement 1: a kind of FED is with the manufacture method of blue luminescent phosphor, and the method is according to following steps:
(1) preparation 1000ppm concentration silver powder: 10kg zinc sulphide is paved in the fine aluminium plate; The 10g Silver Nitrate is dissolved in behind the 1000ml glass beaker to filter with 150 eye mesh screens with pure water fully obtains Silver Nitrate filtrate; Add Silver Nitrate filtrate and pure water in the zinc sulphide and be uniformly mixed into mixture; Mixture is carried out sieving with 150 eye mesh screens after the drying, obtain 1000ppm concentration silver powder, wherein 130 ℃ of drying temperatures, 12 hours time of drying;
(2) fluorescent material batching: zinc sulphide, 1000ppm concentration silver powder, γ-Al
2O
3, barium iodide and sulphur is 100: 30: 0.02715 according to mass percent: 0.125: 3 ratio mixed grinding phosphor mixture, phosphor mixture mix 40min and obtain the fluorescent material batching in mixer after 100 eye mesh screens sieve;
(3) fluorescent material charging sintering: with the 1.0kg fluorescent material batching quartz crucible of packing into; The sulphur of packing in quartz boat bottom, sulfur consumption be in the quartz crucible fluorescent material batching quality 20%, the tight gac that covers on sulphur, activated carbon dosage be in the quartz crucible fluorescent material batching quality 20%; Then quartz boat is placed on the surface of fluorescent material batching, covers tightly quartz crucible; The quartz crucible that covers tightly sintering in the electric stove of nitrogen protection is obtained pure phosphor, and sintering temperature is that 950 ℃, sintering time are 2.5 hours, and adopting agglomerating plant is to burn till in the electric stove in continuous self acting tunnel;
(4) fluorescent material pre-treatment: get rid of under ultraviolet lamp that not luminous or luminous unusual powder obtains qualified pure phosphor in the pure phosphor; Qualified pure phosphor descended 150 eye mesh screen after washings to obtain phosphor slurry in the flushing of pure water; The pure water consumption is 10 times of fluorescent material quality in the described washing, and washing times is 6 times, washes churning time 10min at every turn;
(5) top coat is processed: after phosphor slurry is stirred 10min, in phosphor slurry, be the potassium silicate solution of 24.8-25.2% according to adding the 10ml concentration of volume percent in every kilogram of fluorescent material, and SiO in the potassium silicate solution
2And K
2The mol ratio of O is 3.05; And then stirring the solution of zinc sulfate that adds 0.7 mole behind the 10min, the solution of zinc sulfate consumption is that every kilogram of fluorescent material uses 60ml, last restir 10min; Phosphor slurry after obtaining processing;
(6) preparation blue luminescent phosphor: the phosphor slurry after will processing anhydrates, drying, sieve, and obtains blue luminescent phosphor; The drying temperature of described drying is that 120 ℃, time of drying are 6 hours; Described sieving was the 300-500 eye mesh screen.
Described γ-Al
2O
3Purity 〉=99%, specific surface area is 85～115m
2/ g, pH value are 4.5～5.5 (4% aqueous solution tests), γ-Al
2O
3Middle Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%;
The purity of described barium iodide 〉=99%, the water-insoluble in the barium iodide≤0.01%, muriate and bromide 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%.
The purity of described sulphur＞99.5%, Fe content≤0.3ppm, Pb content≤0.5ppm, Ni content≤0.5ppm in the sulphur.
Described gac is the coconut husk charcoal.
Anhydrating in the described step (6) is to adopt water extracter or vacuum filtration to anhydrate.
Described screen cloth is nylon screen.
Implement 2: a kind of FED is with the manufacture method of blue luminescent phosphor, and the method is according to following steps:
(1) preparation 1000ppm concentration silver powder: 10kg zinc sulphide is paved in the fine aluminium plate; The 10g Silver Nitrate is dissolved in behind the 1000ml glass beaker to filter with 150 eye mesh screens with pure water fully obtains Silver Nitrate filtrate; Add Silver Nitrate filtrate and pure water in the zinc sulphide and be uniformly mixed into mixture; Mixture is carried out sieving with 150 eye mesh screens after the drying, obtain 1000ppm concentration silver powder, wherein 130 ℃ of drying temperatures, 12 hours time of drying;
(2) fluorescent material batching: zinc sulphide, 1000ppm concentration silver powder, γ-Al
2O
3, barium iodide and sulphur is 100: 50: 0.0565 according to mass percent: 0.175: 8 ratio mixed grinding phosphor mixture, phosphor mixture mix 80min and obtain the fluorescent material batching in mixer after 100 eye mesh screens sieve;
(3) fluorescent material charging sintering: with the 2.0kg fluorescent material batching quartz crucible of packing into; The sulphur of packing in quartz boat bottom, sulfur consumption be in the quartz crucible fluorescent material batching quality 30%, the tight gac that covers on sulphur, activated carbon dosage be in the quartz crucible fluorescent material batching quality 30%; Then quartz boat is placed on the surface of fluorescent material batching, covers tightly quartz crucible; The quartz crucible that covers tightly sintering in the electric stove of nitrogen protection is obtained pure phosphor, and sintering temperature is that 970 ℃, sintering time are 2 hours, and adopting agglomerating plant is to burn till in the electric stove in continuous self acting tunnel;
(4) fluorescent material pre-treatment: get rid of under ultraviolet lamp that not luminous or luminous unusual powder obtains qualified pure phosphor in the pure phosphor; Qualified pure phosphor descended 150 eye mesh screen after washings to obtain phosphor slurry in the flushing of pure water; The pure water consumption is 10 times of fluorescent material quality in the described washing, and washing times is 6 times, washes churning time 15min at every turn;
(5) top coat is processed: after phosphor slurry is stirred 15min, in phosphor slurry, be the potassium silicate solution of 24.8-25.2% according to adding the 10ml concentration of volume percent in every kilogram of fluorescent material, and SiO in the potassium silicate solution
2And K
2The mol ratio of O is 3.05; And then stirring the solution of zinc sulfate that adds 0.7 mole behind the 15min, the solution of zinc sulfate consumption is that every kilogram of fluorescent material uses 60ml, last restir 15min; Phosphor slurry after obtaining processing;
(6) preparation blue luminescent phosphor: the phosphor slurry after will processing anhydrates, drying, sieve, and obtains blue luminescent phosphor; The drying temperature of described drying is that 120 ℃, time of drying are 8 hours; Described sieving was 500 eye mesh screens.
Described γ-Al
2O
3Purity 〉=99%, specific surface area is 85～115m
2/ g, pH value are 4.5～5.5 (4% aqueous solution tests), γ-Al
2O
3Middle Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%;
The purity of described barium iodide 〉=99%, the water-insoluble in the barium iodide≤0.01%, muriate and bromide 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%.
The purity of described sulphur＞99.5%, Fe content≤0.3ppm, Pb content≤0.5ppm, Ni content≤0.5ppm in the sulphur.
Described gac is the coconut husk charcoal.
Anhydrating in the described step (6) is to adopt water extracter or vacuum filtration to anhydrate.
Described screen cloth is nylon screen.
Implement 3: a kind of FED is with the manufacture method of blue luminescent phosphor, and the method is according to following steps:
(1) preparation 1000ppm concentration silver powder: 10kg zinc sulphide is paved in the fine aluminium plate; The 10g Silver Nitrate is dissolved in behind the 1000ml glass beaker to filter with 150 eye mesh screens with pure water fully obtains Silver Nitrate filtrate; Add Silver Nitrate filtrate and pure water in the zinc sulphide and be uniformly mixed into mixture; Mixture is carried out sieving with 150 eye mesh screens after the drying, obtain 1000ppm concentration silver powder, wherein 130 ℃ of drying temperatures, 12 hours time of drying;
(2) fluorescent material batching: zinc sulphide, 1000ppm concentration silver powder, γ-Al
2O
3, barium iodide and sulphur is 100: 50: 0.0465 according to mass percent: 0.15: 10 ratio mixed grinding phosphor mixture, phosphor mixture mix 100min and obtain the fluorescent material batching in mixer after 100 eye mesh screens sieve;
(3) fluorescent material charging sintering: with the 1.5kg fluorescent material batching quartz crucible of packing into; The sulphur of packing in quartz boat bottom, sulfur consumption be in the quartz crucible fluorescent material batching quality 25%, the tight gac that covers on sulphur, activated carbon dosage be in the quartz crucible fluorescent material batching quality 25%; Then quartz boat is placed on the surface of fluorescent material batching, covers tightly quartz crucible; The quartz crucible that covers tightly sintering in the electric stove of nitrogen protection is obtained pure phosphor, and sintering temperature is that 9750 ℃, sintering time are 3 hours, and adopting agglomerating plant is to burn till in the electric stove in continuous self acting tunnel;
(4) fluorescent material pre-treatment: get rid of under ultraviolet lamp that not luminous or luminous unusual powder obtains qualified pure phosphor in the pure phosphor; Qualified pure phosphor descended 150 eye mesh screen after washings to obtain phosphor slurry in the flushing of pure water; The pure water consumption is 10 times of fluorescent material quality in the described washing, and washing times is 6 times, washes churning time 12min at every turn;
(5) top coat is processed: after phosphor slurry is stirred 12min, in phosphor slurry, be 25% potassium silicate solution according to adding the 10ml concentration of volume percent in every kilogram of fluorescent material, and SiO in the potassium silicate solution
2And K
2The mol ratio of O is 3.05; And then stirring the solution of zinc sulfate that adds 0.7 mole behind the 12min, the solution of zinc sulfate consumption is that every kilogram of fluorescent material uses 60ml, last restir 12min; Phosphor slurry after obtaining processing;
(6) preparation blue luminescent phosphor: the phosphor slurry after will processing anhydrates, drying, sieve, and obtains blue luminescent phosphor; The drying temperature of described drying is that 120 ℃, time of drying are 6 hours; Described sieving was 400 eye mesh screens.
Described γ-Al
2O
3Purity 〉=99%, specific surface area is 85～115m
2/ g, pH value are 4.5～5.5 (4% aqueous solution tests), γ-Al
2O
3Middle Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%;
The purity of described barium iodide 〉=99%, the water-insoluble in the barium iodide≤0.01%, muriate and bromide 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%.
The purity of described sulphur＞99.5%, Fe content≤0.3ppm, Pb content≤0.5ppm, Ni content≤0.5ppm in the sulphur.
Described gac is the coconut husk charcoal.
Anhydrating in the described step (6) is to adopt water extracter or vacuum filtration to anhydrate.
Described screen cloth is nylon screen.
Above content is in conjunction with concrete preferred implementation further description made for the present invention; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by claims of submitting to.
Claims (6)
1. a FED is characterized in that with the manufacture method of blue luminescent phosphor, and the method is according to following steps:
(1) preparation 1000ppm concentration silver powder: 10kg zinc sulphide is paved in the fine aluminium plate; The 10g Silver Nitrate is dissolved in behind the 1000ml glass beaker to filter with 150 eye mesh screens with pure water fully obtains Silver Nitrate filtrate; Add Silver Nitrate filtrate and pure water in the zinc sulphide and be uniformly mixed into mixture; Mixture is carried out sieving with 150 eye mesh screens after the drying, obtain 1000ppm concentration silver powder, wherein 130 ℃ of drying temperatures, 10-14 hour time of drying;
(2) fluorescent material batching: zinc sulphide, 1000ppm concentration silver powder, γ-Al
2O
3, barium iodide and sulphur is the ratio mixed grinding phosphor mixture of 100:20-60:0.02715-0.0565:0.10-0.20:2.5-12 according to mass percent, phosphor mixture mixes 30-120min and obtains the fluorescent material batching in mixer after 100 eye mesh screens sieve;
(3) fluorescent material charging sintering: with the 1.0-2.0kg fluorescent material batching quartz crucible of packing into; The sulphur of packing in quartz boat bottom, sulfur consumption is the 20-30% of fluorescent material batching quality in the quartz crucible, the tight gac that covers on sulphur, activated carbon dosage is the 20-30% of fluorescent material batching quality in the quartz crucible; Then quartz boat is placed on the surface of fluorescent material batching, covers tightly quartz crucible; The quartz crucible that covers tightly sintering in the electric stove of nitrogen protection is obtained pure phosphor, and sintering temperature is that 950～980 ℃, sintering time are 2-4 hour;
(4) fluorescent material pre-treatment: get rid of under ultraviolet lamp that not luminous or luminous unusual powder obtains qualified pure phosphor in the pure phosphor; Qualified pure phosphor descended 150 eye mesh screen after washings to obtain phosphor slurry in the flushing of pure water; The pure water consumption is 10 times of fluorescent material quality in the described washing, and washing times is 6 times, washes churning time 10-15min at every turn;
(5) top coat is processed: after phosphor slurry is stirred 10-15min, in phosphor slurry, be the potassium silicate solution of 24.8-25.2% according to adding the 10ml concentration of volume percent in every kilogram of fluorescent material, and SiO in the potassium silicate solution
2And K
2The mol ratio of O is 3.05; And then stirring the solution of zinc sulfate that adds 0.7 mole behind the 10-15min, the solution of zinc sulfate consumption is that every kilogram of fluorescent material uses 60ml, last restir 10-15min; Phosphor slurry after obtaining processing;
(6) preparation blue luminescent phosphor: the phosphor slurry after will processing anhydrates, drying, sieve, and obtains blue luminescent phosphor; The drying temperature of described drying is that 110-130 ℃, time of drying are 4-8 hour; Described sieving was the 300-500 eye mesh screen.
2. described a kind of FED is characterized in that: described γ-Al with the manufacture method of blue luminescent phosphor according to claim 1
2O
3Purity 〉=99%, γ-Al
2O
3Specific surface area be 85～115m
2/ g, pH value are 4.5～5.5, Fe content≤5ppm, Pb content≤5ppm, Ni content≤3ppm, SO
4 2-≤ 0.005%, burning decrement≤1%.
3. described a kind of FED is characterized in that: the purity of described sulphur with the manufacture method of blue luminescent phosphor according to claim 1〉99.5%, Fe content≤0.3ppm, Pb content≤0.5ppm, Ni content≤0.5ppm in the sulphur.
4. described a kind of FED is with the manufacture method of blue luminescent phosphor according to claim 1, and it is characterized in that: described gac is the coconut husk charcoal.
5. described a kind of FED is with the manufacture method of blue luminescent phosphor according to claim 1, and it is characterized in that: anhydrating in the described step (6) is to adopt water extracter or vacuum filtration to anhydrate.
6. described a kind of FED is with the manufacture method of blue luminescent phosphor according to claim 1, and it is characterized in that: described screen cloth is nylon screen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910022660 CN101591532B (en) | 2009-05-22 | 2009-05-22 | Method for preparing blue luminescent phosphor for FED |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910022660 CN101591532B (en) | 2009-05-22 | 2009-05-22 | Method for preparing blue luminescent phosphor for FED |
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| Publication Number | Publication Date |
|---|---|
| CN101591532A CN101591532A (en) | 2009-12-02 |
| CN101591532B true CN101591532B (en) | 2013-01-02 |
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ID=41406415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910022660 Expired - Fee Related CN101591532B (en) | 2009-05-22 | 2009-05-22 | Method for preparing blue luminescent phosphor for FED |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352243B (en) * | 2011-07-22 | 2014-02-12 | 彩虹集团电子股份有限公司 | Preparation method of blue luminescent phosphor for FED |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4975619A (en) * | 1988-12-21 | 1990-12-04 | Rca Licensing Corp. | Surface treatment of silica-coated phosphor particles and method for a CRT screen |
| CN101270284A (en) * | 2008-04-29 | 2008-09-24 | 彩虹集团电子股份有限公司 | Method for preparing blue-fluorescence body for cold cathode fluorescent lamp |
| CN101376806A (en) * | 2008-10-13 | 2009-03-04 | 彩虹集团电子股份有限公司 | Preparation of blue powder for color display tube |
-
2009
- 2009-05-22 CN CN 200910022660 patent/CN101591532B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4975619A (en) * | 1988-12-21 | 1990-12-04 | Rca Licensing Corp. | Surface treatment of silica-coated phosphor particles and method for a CRT screen |
| CN101270284A (en) * | 2008-04-29 | 2008-09-24 | 彩虹集团电子股份有限公司 | Method for preparing blue-fluorescence body for cold cathode fluorescent lamp |
| CN101376806A (en) * | 2008-10-13 | 2009-03-04 | 彩虹集团电子股份有限公司 | Preparation of blue powder for color display tube |
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| CN101591532A (en) | 2009-12-02 |
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