CN101434404A - Preparation of europium gadolinium yttrium oxide red fluorescent powder - Google Patents
Preparation of europium gadolinium yttrium oxide red fluorescent powder Download PDFInfo
- Publication number
- CN101434404A CN101434404A CN 200810232745 CN200810232745A CN101434404A CN 101434404 A CN101434404 A CN 101434404A CN 200810232745 CN200810232745 CN 200810232745 CN 200810232745 A CN200810232745 A CN 200810232745A CN 101434404 A CN101434404 A CN 101434404A
- Authority
- CN
- China
- Prior art keywords
- fluorescent powder
- red fluorescent
- yttrium oxide
- powder
- oxide red
- 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 preparation method of yttria gadolinium-europium red fluorescent powder, which comprises the steps of: mixing 60-80 weight percent of Y2O3, 10-40 weight percent of Gd2O3 and 1-10 weight percent of Eu2O3 by a dry method after the materials are screened by a 100-mesh screen, putting the uniformly mixed materials in a crucible, firing the materials for 4-10 hours under the high temperature of 900-1400 DEG C, screening the fired fluorescent powder blocks by the 100-mesh screen, scattering the powder into slurry by a wet method, washing the scattered slurry for 2-5 times, then filtering and drying the slurry for 8-24 hours at 110-120 DEG C, and screening the dried powder by the 100-mesh screen to obtain the yttria gadolinium-europium red fluorescent powder.
Description
Technical field
The present invention relates to a kind of preparation method of red fluorescence powder, particularly a kind of preparation method of burst of ultraviolel europium gadolinium yttrium oxide red fluorescent powder.
Background technology
Burst of ultraviolel Y
2O
3: what the Eu formula was represented is a kind of red fluorescence powder, and the research of yttrium europium oxide red fluorescence powder is had for a long time history, wherein relates to high temperature solid phase synthesis, sol-gel method, combustion synthesis method and microwave process for synthesizing.Simple owing to high temperature solid phase synthesis equipment at present, stable processing technique, yield is high and most widely used general.In recent years, along with technology rapid development, the yttrium europium oxide red fluorescence powder is good owing to luminosity height under vacuum-ultraviolet light, colour purity, stable to be widely used.Commercial at present yttrium europium oxide ubiquity excites down in certain temperature and high capacity, and the powder decay of luminescence is very fast, the problem that the colourity drift is bigger.
Summary of the invention
The object of the present invention is to provide a kind of preparation method that can be applicable to the europium gadolinium yttrium oxide red fluorescent powder under high temperature, high pressure, the high capacity, make to produce red fluorescence powder to have a particle diameter changeable that brightness height, light decay, look float little characteristics.
For achieving the above object, the present invention takes following technical scheme to be achieved:
A kind of preparation method of europium gadolinium yttrium oxide red fluorescent powder comprises the steps:
Step 1: the Y that takes by weighing 60-80% by mass percentage
2O
3, 10-40% Gd
2O
3, 1-10% Eu
2O
3Dry mixed, each raw material is crossed 100 mesh sieves before mixing;
Step 2: with the powder that mixes under 900-1400 ℃ high temperature calcination 4-10 hour;
Step 3: the fluorescence powder piece that burns till is pulverized the back cross 100 mesh sieves, wet method is dispersed into slurry;
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, suction filtration, dry screening promptly get europium gadolinium yttrium oxide red fluorescent powder then.
In the aforesaid method, the described dry mixed of step 1 is that each raw material that sieves is packed in the ball grinder, and with material: ball is that the part by weight of 2:1 mixes, and the diameter of ball is 1cm, ball milling 12-48 hour.It is in ball grinder that the described wet method of step 3 is disperseed, by material: water: disperse ball be the quality of 1:2:2 than ball milling 0.5-5 hour, disperseing the diameter of ball is 1.5-2.5mm.The described dry screening of step 4 is under 110-120 ℃ temperature dry 8-24 hour, and after 100 mesh sieves, the granular size of the gained europium gadolinium yttrium oxide red fluorescent powder that sieves is 2-7um.
The material of existing ultraviolet excitated red fluorescent powder is formed yttrium oxide, europium sesquioxide system, and its excitation principle is to be activator with the europium.Contain a certain amount of gadolinium sesquioxide in the component of fluorescent material of the present invention, can make and burn till the speed of reaction raising, react more abundant, make Eu
3+Can as much as possiblely enter the yttrium oxide lattice, thereby form more more stable luminescence center, improve the luminous intensity of yttrium europium oxide, and strengthen sustainment rate greatly.By a certain amount of gadolinium sesquioxide that mixes, can also in burning till, change crystal morphology, make this powder performance on using improve, can improve the coating effect, mixing when using with other fluorescent material, can have better membranous, thereby further improve light efficiency.
The europium gadolinium yttrium oxide red fluorescent powder that adopts the inventive method to obtain has high brightness, colour purity is good, light decay is little advantage.
Embodiment
Embodiment 1
At first be 60% Y with mass percent
2O
3, 39% Gd
2O
3, 1% Eu
2O
3Drop in the batch mixing bottle after crossing earlier 100 mesh sieves, with powder: ball is the mixed of 2:1, and the diameter of ball is that 1-5cm distributes, and ball milling 18 hours promptly gets the fluorescent material starting material that mix.The raw material of the fluorescent material that mixes is put into alumina crucible, alumina crucible is put into the high temperature firing furnace, calcination is 10 hours under 900 ℃ high temperature, cooledly burns till the primary product that product promptly are this red fluorescence powders.100 mesh sieves will be crossed after the fluorescent material powder agglomates fragmentation of burning till, drop in the ball grinder, with powder: water: disperse ball press the mass ratio mixing of 1:2:2, the dispersion spherical diameter is 1.5-2.5mm, Ball milling through 0.5 hour, the powder that ball milling is dismissed was starched 500 mesh sieves, removed the screening reject on 500 eye mesh screens, and scattered powder slurry is through 3 washings, suction filtration then, drying is 12 hours under 110 ℃ temperature, and dry good powder is crossed 100 mesh sieves, promptly gets red fluorescence powder.This powder brightness 95, granularity 6.8u.
Embodiment 2
At first be 68% Y with mass percent
2O
3, 30% Gd
2O
3, 2% Eu
2O
3Pressing the method for embodiment 1 mixed 12 hours, and put into firing furnace, calcination is 8 hours under 1000 ℃ high temperature, the cooled product that burn till were by the method Ball milling of embodiment 1 1.0 hours, scattered powder slurry is through 3 washings, suction filtration then, under 120 ℃ temperature dry 8 hours, dry good powder is crossed 100 mesh sieves, promptly gets this red fluorescence powder.This powder brightness 98, granularity 6.2u.
Embodiment 3
At first be 70% Y with mass percent
2O
3, 27% Gd
2O
3, 3% Eu
2O
3Pressing the method for embodiment 1 mixed 20 hours, and put into firing furnace, calcination is 7 hours under 1100 ℃ high temperature, the cooled product that burn till were by the method Ball milling of embodiment 1 1.5 hours, scattered powder slurry is through 2 washings, suction filtration then, under 110 ℃ temperature dry 14 hours, dry good powder is crossed 100 mesh sieves, promptly gets this red fluorescence powder.This powder brightness 101, granularity 5.8u.
Embodiment 4
At first be 71% Y with mass percent
2O
3, 25% Gd
2O
3, 4% Eu
2O
3Pressing the method for embodiment 1 mixed 24 hours, and put into firing furnace, calcination is 6 hours under 1200 ℃ high temperature, the cooled product that burn till were by the method Ball milling of embodiment 1 2.0 hours, scattered powder slurry is through 3 washings, suction filtration then, under 110 ℃ temperature dry 16 hours, dry good powder is crossed 100 mesh sieves, promptly gets this red fluorescence powder.This powder brightness 104, granularity 5.5u.
Embodiment 5
At first be 72% Y with mass percent
2O
3, 23% Gd
2O
3, 5% Eu
2O
3Pressing the method for embodiment 1 mixed 36 hours, and put into firing furnace, calcination is 5 hours under 1300 ℃ high temperature, the cooled product that burn till were by the method Ball milling of embodiment 1 3.0 hours, scattered powder slurry is through 4 washings, suction filtration then, under 110 ℃ temperature dry 20 hours, dry good powder is crossed 100 mesh sieves, promptly gets this red fluorescence powder.This powder brightness 106, granularity 5.0u.
Embodiment 6
At first be 80% Y with mass percent
2O
3, 10% Gd
2O
3, 10% Eu
2O
3Pressing the method for embodiment 1 mixed 48 hours, and put into firing furnace, calcination is 4 hours under 1400 ℃ high temperature, the cooled product that burn till were by the method Ball milling of embodiment 15 hours, scattered powder slurry is through 5 washings, suction filtration then, under 110 ℃ temperature dry 24 hours, dry good powder is crossed 100 mesh sieves, promptly gets this red fluorescence powder.This powder brightness 107, granularity 4.7u.
Claims (6)
1, a kind of preparation method of europium gadolinium yttrium oxide red fluorescent powder is characterized in that, comprises the steps:
Step 1: the Y that takes by weighing 60-80% by mass percentage
2O
3, 10-40% Gd
2O
3, 1-10% Eu
2O
3Dry mixed, each raw material is crossed 100 mesh sieves before mixing;
Step 2: with the powder that mixes under 900-1400 ℃ high temperature calcination 4-10 hour;
Step 3: the fluorescence powder piece that burns till is pulverized the back cross 100 mesh sieves, wet method is dispersed into slurry;
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, suction filtration, dry screening promptly get europium gadolinium yttrium oxide red fluorescent powder then.
2, the preparation method of europium gadolinium yttrium oxide red fluorescent powder as claimed in claim 1 is characterized in that, the described dry mixed of step 1 is that each raw material that sieves is packed in the ball grinder, and with material: ball is that the part by weight of 2:1 mixes ball milling 12-48 hour.
3, the preparation method of europium gadolinium yttrium oxide red fluorescent powder as claimed in claim 2 is characterized in that, the diameter of described ball is 1-5cm.
4, the preparation method of europium gadolinium yttrium oxide red fluorescent powder as claimed in claim 1 is characterized in that, it is in ball grinder that the described wet method of step 3 is disperseed, and by material: water: disperseing ball is that the quality of 1:2:2 was than ball milling 0.5-5 hour.
5, the preparation method of europium gadolinium yttrium oxide red fluorescent powder as claimed in claim 4 is characterized in that, the diameter of described dispersion ball is 1.5-2.5mm.
6, the preparation method of europium gadolinium yttrium oxide red fluorescent powder as claimed in claim 1, it is characterized in that, the described dry screening of step 4 is under 110-120 ℃ temperature dry 8-24 hour, and after 100 mesh sieves, the granular size of the gained europium gadolinium yttrium oxide red fluorescent powder that sieves is 2-7um.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810232745 CN101434404A (en) | 2008-12-09 | 2008-12-09 | Preparation of europium gadolinium yttrium oxide red fluorescent powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810232745 CN101434404A (en) | 2008-12-09 | 2008-12-09 | Preparation of europium gadolinium yttrium oxide red fluorescent powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101434404A true CN101434404A (en) | 2009-05-20 |
Family
ID=40709064
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200810232745 Pending CN101434404A (en) | 2008-12-09 | 2008-12-09 | Preparation of europium gadolinium yttrium oxide red fluorescent powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101434404A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344805A (en) * | 2010-08-03 | 2012-02-08 | 三星Sdi株式会社 | Red phosphor and plasma display panel including same |
| CN106635005A (en) * | 2016-06-13 | 2017-05-10 | 郑甘裕 | Europium-doped gadolinium oxide luminescent material as well as preparation method and application thereof |
-
2008
- 2008-12-09 CN CN 200810232745 patent/CN101434404A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344805A (en) * | 2010-08-03 | 2012-02-08 | 三星Sdi株式会社 | Red phosphor and plasma display panel including same |
| CN106635005A (en) * | 2016-06-13 | 2017-05-10 | 郑甘裕 | Europium-doped gadolinium oxide luminescent material as well as preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107285746A (en) | A kind of preparation method and fluorescence associated ceramics of the fluorescence ceramics of alumina host | |
| CN104130778B (en) | superfine fluorescent powder preparation method | |
| CN101445729B (en) | Preparation method of phosphor powder for white LED | |
| WO2013177848A1 (en) | Silica-coated orange-red fluorescent powder and preparation method thereof | |
| CN102051171B (en) | Method for preparing low-europium red fluorescent powder | |
| CN102352250B (en) | Method for preparing green gadolinium terbium oxysulfide phosphor | |
| CN101434404A (en) | Preparation of europium gadolinium yttrium oxide red fluorescent powder | |
| Manohar et al. | Photoluminescence Studies of Rare-Earth-Doped (Ce3+) LaAlO3 nanopowders prepared by facile combustion route | |
| CN102559189A (en) | Blue fluorescent powder and preparation method thereof | |
| CN102888224A (en) | Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor | |
| CN102337129A (en) | Red luminescent fluorescent powder for FED (Field Emission Display) 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 | |
| CN102337122B (en) | Silicate green fluorescent powder and preparation method thereof | |
| CN101586029B (en) | Yttrium-gadolinium-europium borate red phosphors and preparation method thereof | |
| CN102888223A (en) | Manufacture method for red fluorescent powder for three-primary-color energy saving lamp | |
| CN100554363C (en) | A kind of manufacture method of superfine fluorescent powder | |
| CN101434837B (en) | Ultraviolet excitated red fluorescent powder surface treating method | |
| CN102888219A (en) | Method for preparing rare-earth aluminate blue-green fluorescent powder for energy-saving lamp | |
| CN106010528A (en) | Bismuth-manganese-doped blue fluorescent powder and preparation method and application thereof | |
| CN105838371A (en) | Nitric oxide fluorescent powder for LED and preparation method | |
| CN101619215A (en) | Red fluorescent powder excited by ultraviolet light and blue light and preparation method thereof | |
| CN101696356B (en) | Method for manufacturing borate green phosphor | |
| CN101168668A (en) | Method for manufacturing green phosphor used for color plasma | |
| CN101705093A (en) | Manufacturing method of blue-green fluorescent powder used for high-color developing energy-saving lamp |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090520 |