CN102888224A - Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor - Google Patents
Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor Download PDFInfo
- Publication number
- CN102888224A CN102888224A CN201210331274XA CN201210331274A CN102888224A CN 102888224 A CN102888224 A CN 102888224A CN 201210331274X A CN201210331274X A CN 201210331274XA CN 201210331274 A CN201210331274 A CN 201210331274A CN 102888224 A CN102888224 A CN 102888224A
- Authority
- CN
- China
- Prior art keywords
- ball
- mesh sieves
- hours
- wet method
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses a method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor. The method comprises the following steps of: weighing Al2O3, MgO, Tb3O4 and CeO2 in a mass ratio, sieving all raw materials by using a 100-mesh sieve, mixing by a dry method, introducing one or more of BaCO3, MgCl2, AlF3, MgF2, BaF2 and H3BO3 into the uniformly mixed raw materials, and fully mixing; loading the mixed powder into an alumina crucible; firing at high temperature at reducing atmosphere; crushing the fired fluorescent powder blocks, and sieving by using the 100-mesh sieve; dispersing by a wet method to obtain slurry; controlling the particle size to be 2 to 12 mu m; sieving the slurry which is obtained by wet-method dispersing by using a 500-mesh sieve; removing the sieving residues on the 500-mesh sieve; washing with water; and suction-filtering, drying and screening to obtain the green emitting phosphor. The green emitting phosphor has the characteristics of controllable particle size, high brightness, light failure, color development and low color bleaching.
Description
Technical field
The present invention relates to a kind of preparation method of green emitting phosphor, particularly the preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor.
Background technology
Burst of ultraviolel or vacuum ultraviolet-excited CeMgAl
11O
19: what the Tb formula represented is a kind of green emitting phosphor, wherein relates to high temperature solid phase synthesis, sol-gel method, combustion synthesis method and microwave process for synthesizing.Mostly be high temperature oxidation, low-temperature reduction solid-phase synthesis in the existing market, but this technical matters is comparatively loaded down with trivial details, the difficult control of process complex product quality, and product yield is low, and production cost is high, in recent years, along with developing rapidly of technology, CeMgAl
11O
19: the Tb green emitting phosphor has begun to be applied to display device with in the backlight assembly, but adopt product that traditional technology produces light efficiency, the problem such as brightness is on the low side, light decay, colour developing and colourity drift are larger under vacuum-ultraviolet light, demand that can not satisfying the market.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide the preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor, producing green emitting phosphor, to have a particle diameter changeable, and brightness is high, light decay, colour developing, look float little characteristics.
For achieving the above object, the present invention takes following technical scheme to be achieved:
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing α or the MgO of β-Al2O3,1-10%, the Tb of 1-10% of 70-80% by mass percentage
3O
4, 1-20% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 0.1-10 ‰ in the starting material that mix
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3In one or several fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 12-48 hour;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, under 900-1500 ℃ high-temperature reductibility atmosphere calcination 4-10 hour;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 2-12 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 0.5-5 hour, and disperseing the diameter of ball is 1.5-3.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 2-5 washing, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110-120 ℃ temperature dry 8-24 hour, and after 200 mesh sieves, the granular size of this green emitting phosphor of gained that sieves is 2-12 μ m.
The material of existing burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor forms aluminum oxide, magnesium oxide, cerium oxide, terbium sesquioxide system, and its excitation principle is take cerium as sensitizing agent, and terbium is activator, by a kind of green emitting phosphor of transmission ofenergy.Contain a certain amount of BaCO in the component of fluorescent material of the present invention
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3, at CeMgAl
11O
19: in the Tb sintering, a certain amount of BaCO mixes
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3, can make and burn till the speed of reaction raising, react more abundant, make Tb
3+Can as much as possiblely enter magnesium aluminate cerium lattice, thereby form more more stable luminescence center, improve at a certain temperature, the luminous intensity of magnesium aluminate cerium terbium, and greatly strengthen sustainment rate, by a certain amount of BaCO that mixes
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3Middle change crystal morphology can also burnt till, so that this powder performance on application characteristic improves, can better be applied in the larger vacuum ultraviolet-excited display device of excitation energy, when mixing use with other fluorescent material, can have better membranous, thereby further improve light efficiency, improve colour developing and purity of color.Obtain high brightness, colour purity is good, light decay is little burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor, at first will in magnesium aluminate cerium terbium, introduce a certain amount of BaCO
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3, after mixing, reductive firing just can obtain this powder, BaCO at a certain temperature
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3What of introducing amount have a significant impact the effect that powder burns till, and quantitative BaCO mixes
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3Powder sintering can be more complete, and crystal morphology is mellow and full full, and the powder characteristics of luminescence can be greatly improved, and its Application Areas also can enlarge, and firing temperature also can affect BaCO
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3Doping effect in magnesium aluminate cerium terbium, under the certain temperature, BaCO
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3Can better be combined with aluminum oxide, magnesium oxide, cerium oxide, terbium sesquioxide, in application, improve the powder anti-decay property, make luminous efficacy better.
Embodiment
Below in conjunction with specific embodiment the present invention is described in detail.
Embodiment 1
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 70% α-Al2O3,3% MgO, 9% Tb by mass percentage
3O
4, 18% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 10 ‰ in the starting material that mix
3, MgCl
2Solution fully mixes,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 12-48 hour;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 10 hours under 900 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 12 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 0.5 hour, and disperseing the diameter of ball is 1.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 3 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 12 hours, after 200 mesh sieves.After measured, this green emitting phosphor brightness 95%, granularity 12 μ m.
Embodiment 2
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 72% β-Al2O3,4% MgO, 8% Tb by mass percentage
3O
4, 16% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 8 ‰ in the starting material that mix
3, MgCl
2, AlF
3, MgF
2Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 20 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 8 hours under 1000 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 10 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 1.0 hours, and disperseing the diameter of ball is 2.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 3 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 120 ℃ temperature dry 8 hours, after 200 mesh sieves.After measured, this green emitting phosphor brightness 98%, granularity 10 μ m.
Embodiment 3
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 74% α-Al2O3,5% MgO, 7% Tb by mass percentage
3O
4, 14% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the MgF of raw material quality 6 ‰ in the starting material that mix
2, BaF
2Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 20 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 7 hours under 1100 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 9 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 2.0 hours, and disperseing the diameter of ball is 2.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 3 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 14 hours, after 200 mesh sieves.
After measured, this green emitting phosphor.This powder brightness 101%, granularity 9 μ m.
Embodiment 4
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 75% β-Al2O3,5% MgO, 6% Tb by mass percentage
3O
4, 14% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the MgCl of raw material quality 5 ‰ in the starting material that mix
2, BaF
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 24 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 3.0 hours under 1200 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 8 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 0.5-5 hour, and disperseing the diameter of ball is 3.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 4 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 115 ℃ temperature dry 16 hours, after 200 mesh sieves.
After measured, the brightness 105% of this green emitting phosphor, granularity 8 μ m.
Embodiment 5
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 76% α-Al2O3,6% MgO, 5% Tb by mass percentage
3O
4, 13% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 4 ‰ in the starting material that mix
3, MgCl
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 36 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 5 hours under 1300 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 7 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 4.0 hours, and disperseing the diameter of ball is 2.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 4 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 20 hours, after 200 mesh sieves.
After measured, this green emitting phosphor brightness 106%, granularity 7 μ m.
Embodiment 6
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 77% α-Al2O3,6% MgO, 7% Tb by mass percentage
3O
4, 10% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 3 ‰ in the starting material that mix
3, MgCl
2, BaF
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 48 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 4 hours under 1400 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 6 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 4.5 hours, and disperseing the diameter of ball is 2.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 5 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 24 hours, after 200 mesh sieves.
After measured, the brightness 107% of this green emitting phosphor, granularity 6 μ.
Embodiment 7
The preparation method of a kind of burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor comprises the steps:
Step 1 takes by weighing 80% β-Al2O3,6% MgO, 6% Tb by mass percentage
3O
4, 8% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 0.1 ‰ in the starting material that mix
3, MgCl
2, BaF
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 48 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 4 hours under 1500 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 2 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 5 hours, and disperseing the diameter of ball is 1.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 5 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 120 ℃ temperature dry 24 hours, after 200 mesh sieves.
After measured, this green emitting phosphor brightness 92%, granularity 2 μ m.
Claims (8)
1. the preparation method of a burst of ultraviolel or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing α or the MgO of β-Al2O3,1-10%, the Tb of 1-10% of 70-80% by mass percentage
3O
4, 1-20% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 0.1-10 ‰ in the starting material that mix
3, MgCl
2, AlF
3, MgF
2, BaF
2, H
3BO
3In one or several fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 12-48 hour;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, under 900-1500 ℃ high-temperature reductibility atmosphere calcination 4-10 hour;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 2-12 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 0.5-5 hour, and disperseing the diameter of ball is 1.5-3.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 2-5 washing, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110-120 ℃ temperature dry 8-24 hour, and after 200 mesh sieves, the granular size of this green emitting phosphor of gained that sieves is 2-12 μ m.
2. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 70% α-Al2O3,3% MgO, 9% Tb by mass percentage
3O
4, 18% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 10 ‰ in the starting material that mix
3, MgCl
2Solution fully mixes,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 12-48 hour;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 10 hours under 900 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 12 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 0.5 hour, and disperseing the diameter of ball is 1.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 3 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 12 hours, after 200 mesh sieves.
3. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 72% β-Al2O3,4% MgO, 8% Tb by mass percentage
3O
4, 16% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 8 ‰ in the starting material that mix
3, MgCl
2, AlF
3, MgF
2Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 20 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 8 hours under 1000 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 10 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 1.0 hours, and disperseing the diameter of ball is 2.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 3 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 120 ℃ temperature dry 8 hours, after 200 mesh sieves.
4. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 74% α-Al2O3,5% MgO, 7% Tb by mass percentage
3O
4, 14% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the MgF of raw material quality 6 ‰ in the starting material that mix
2, BaF
2Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 20 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 7 hours under 1100 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 9 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 2.0 hours, and disperseing the diameter of ball is 2.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 3 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 14 hours, after 200 mesh sieves.
5. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 75% β-Al2O3,5% MgO, 6% Tb by mass percentage
3O
4, 14% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the MgCl of raw material quality 5 ‰ in the starting material that mix
2, BaF
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 24 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 3.0 hours under 1200 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 8 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 0.5-5 hour, and disperseing the diameter of ball is 3.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 4 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 115 ℃ temperature dry 16 hours, after 200 mesh sieves.
6. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 76% α-Al2O3,6% MgO, 5% Tb by mass percentage
3O
4, 13% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 4 ‰ in the starting material that mix
3, MgCl
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 36 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 5 hours under 1300 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 7 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 4.0 hours, and disperseing the diameter of ball is 2.5mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 4 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 20 hours, after 200 mesh sieves.
7. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 77% α-Al2O3,6% MgO, 7% Tb by mass percentage
3O
4, 10% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of raw material quality 3 ‰ in the starting material that mix
3, MgCl
2, BaF
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 48 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 4 hours under 1400 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 6 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 4.5 hours, and disperseing the diameter of ball is 2.0mm;
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 5 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 110 ℃ temperature dry 24 hours, after 200 mesh sieves.
8. the preparation method of a kind of burst of ultraviolel according to claim 1 or vacuum ultraviolet-excited green emitting phosphor is characterized in that, comprises the steps:
Step 1 takes by weighing 80% β-Al2O3,6% MgO, 6% Tb by mass percentage
3O
4, 8% CeO
2Dry mixed, each raw material is crossed 100 mesh sieves before mixing, and introduces the BaCO of starting material 0.1 ‰ in the starting material that mix
3, MgCl
2, BaF
2, H
3BO
3Fully mix,
Described dry mixed is that each raw material that sieves is packed in the ball grinder, and take material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 5cm, ball milling 48 hours;
Step 2, with the powder that the mixes aluminum oxide material crucible of packing into, calcination is 4 hours under 1500 ℃ high-temperature reductibility atmosphere;
Step 3 is pulverized rear 100 mesh sieves of crossing with the fluorescence powder piece that burns till, and wet method is dispersed into slurry, and granularity is controlled at 2 μ m,
It is in ball grinder that described wet method is disperseed, adopt aluminum oxide, agate, glass sphere all can, according to ball: powder: pure water or alcohols ratio are 2:1:2, disperse ball milling 5 hours, and disperseing the diameter of ball is 1.5mm
Step 4, the slurry that wet method is scattered is crossed 500 mesh sieves, removes the screening reject on 500 eye mesh screens, and through 5 washings, then suction filtration, dry screening namely get this green emitting phosphor,
Described dry screening is under 120 ℃ temperature dry 24 hours, after 200 mesh sieves.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210331274XA CN102888224A (en) | 2012-09-07 | 2012-09-07 | Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210331274XA CN102888224A (en) | 2012-09-07 | 2012-09-07 | Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102888224A true CN102888224A (en) | 2013-01-23 |
Family
ID=47531909
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210331274XA Pending CN102888224A (en) | 2012-09-07 | 2012-09-07 | Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102888224A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739153A (en) * | 2017-11-06 | 2018-02-27 | 南昌大学 | A kind of clear glass and preparation method with highly effective green light transmitting |
| CN114606000A (en) * | 2022-03-22 | 2022-06-10 | 陕西彩虹新材料有限公司 | Laser excitation display green phosphor and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3937998A (en) * | 1973-10-05 | 1976-02-10 | U.S. Philips Corporation | Luminescent coating for low-pressure mercury vapour discharge lamp |
| CN85100242A (en) * | 1985-04-01 | 1986-10-15 | 武汉大学 | The synthetic lamp rare earth indigo plant of carbon reduction method, green two kinds of fluorescent material |
| JP2004253190A (en) * | 2003-02-18 | 2004-09-09 | Matsushita Electric Ind Co Ltd | Fluorescent lamp |
| CN101041774A (en) * | 2007-04-25 | 2007-09-26 | 常熟市亚太荧光材料有限公司 | Three primary colors fluorescent powder for cold cathode luminous source and preparation method thereof |
| CN101701153A (en) * | 2009-11-17 | 2010-05-05 | 江门市科恒实业股份有限公司 | Method for preparing aluminate green phosphor with low content of terbium |
| CN101705092A (en) * | 2009-10-30 | 2010-05-12 | 彩虹集团电子股份有限公司 | Manufacturing method of strontium-magnesium-tin phosphate red fluorescent powder used for high-color developing energy-saving lamp |
| CN102373060A (en) * | 2011-10-19 | 2012-03-14 | 江门市科恒实业股份有限公司 | Aluminate green fluorescent powder with core-shell structure and preparation method thereof |
-
2012
- 2012-09-07 CN CN201210331274XA patent/CN102888224A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3937998A (en) * | 1973-10-05 | 1976-02-10 | U.S. Philips Corporation | Luminescent coating for low-pressure mercury vapour discharge lamp |
| CN85100242A (en) * | 1985-04-01 | 1986-10-15 | 武汉大学 | The synthetic lamp rare earth indigo plant of carbon reduction method, green two kinds of fluorescent material |
| JP2004253190A (en) * | 2003-02-18 | 2004-09-09 | Matsushita Electric Ind Co Ltd | Fluorescent lamp |
| CN101041774A (en) * | 2007-04-25 | 2007-09-26 | 常熟市亚太荧光材料有限公司 | Three primary colors fluorescent powder for cold cathode luminous source and preparation method thereof |
| CN101705092A (en) * | 2009-10-30 | 2010-05-12 | 彩虹集团电子股份有限公司 | Manufacturing method of strontium-magnesium-tin phosphate red fluorescent powder used for high-color developing energy-saving lamp |
| CN101701153A (en) * | 2009-11-17 | 2010-05-05 | 江门市科恒实业股份有限公司 | Method for preparing aluminate green phosphor with low content of terbium |
| CN102373060A (en) * | 2011-10-19 | 2012-03-14 | 江门市科恒实业股份有限公司 | Aluminate green fluorescent powder with core-shell structure and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| BYOUNG-KYU PARK ET AL: "Single-Step Solid-State Synthesis of CeMgAl11O19:Tb Phosphor", 《BULL. KOREAN CHEM. SOC.》 * |
| 康凯 等: "铝酸盐绿色荧光粉制备工艺与发光性能关系的研究", 《中国稀土学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739153A (en) * | 2017-11-06 | 2018-02-27 | 南昌大学 | A kind of clear glass and preparation method with highly effective green light transmitting |
| CN114606000A (en) * | 2022-03-22 | 2022-06-10 | 陕西彩虹新材料有限公司 | Laser excitation display green phosphor and preparation method thereof |
| CN114606000B (en) * | 2022-03-22 | 2023-10-13 | 陕西彩虹新材料有限公司 | Laser excitation display green phosphor and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Luminescent properties of Eu3+ and Sm3+ activated M2SiO4 (M= Ba, Sr and Ca) red-emitting phosphors for WLEDs | |
| CN101445729B (en) | Preparation method of phosphor powder for white LED | |
| CN102660284B (en) | Manufacturing method of red nitride fluorescent powder for LED | |
| WO2013177848A1 (en) | Silica-coated orange-red fluorescent powder and preparation method thereof | |
| CN102888224A (en) | Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor | |
| CN105331365B (en) | A kind of preparation method of LED fluorescent powder | |
| Huang et al. | Preparation and near-white luminescence properties of Bi3+ doped and Bi3+/Eu3+ co-doped germanate phosphor powder | |
| CN101397497A (en) | Method for preparing fluorescent powder for white background illuminating source | |
| CN103980901A (en) | Preparation method of YAG:Ce<3+> yellow fluorescent powder for white light LED | |
| CN102585830A (en) | Cerium-activated silicate green fluorescent powder and preparation method thereof | |
| CN101255337B (en) | Preparation method of red-light fluorescent powder for LED or PDP display | |
| CN105176530A (en) | High-brightness tungstate red fluorescent powder and preparation method thereof | |
| CN101586029B (en) | Yttrium-gadolinium-europium borate red phosphors and preparation method thereof | |
| CN101787281A (en) | Europium-activated blue/green light emitting fluorescent powder and preparation method thereof | |
| CN104845615A (en) | Rare-earth doped beta-phase Sr2SiO4 nano-powder and preparation method therefor | |
| CN100500797C (en) | Preparation method of aluminate base blue fluorescent powder | |
| CN101434404A (en) | Preparation of europium gadolinium yttrium oxide red fluorescent powder | |
| CN102337129A (en) | Red luminescent fluorescent powder for FED (Field Emission Display) and preparation method thereof | |
| CN102559189A (en) | Blue fluorescent powder and preparation method thereof | |
| CN102888223A (en) | Manufacture method for red fluorescent powder for three-primary-color energy saving lamp | |
| CN103849386B (en) | A kind of colloidal sol auto-combustion method prepares the method for aluminate blue fluorescent powder | |
| CN102888219A (en) | Method for preparing rare-earth aluminate blue-green fluorescent powder for energy-saving lamp | |
| CN101696356B (en) | Method for manufacturing borate green phosphor | |
| CN102352249A (en) | (Y1-x-yGdy,Eux)(P1-a,Va)O4 red phosphor and preparation method thereof | |
| CN107312529B (en) | Narrow half-peak-width green silicate fluorescent powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130123 |