CN101298559B - Preparation of rare earth tricolor mixing phosphor for CCFL - Google Patents
Preparation of rare earth tricolor mixing phosphor for CCFL Download PDFInfo
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- CN101298559B CN101298559B CN 200810018077 CN200810018077A CN101298559B CN 101298559 B CN101298559 B CN 101298559B CN 200810018077 CN200810018077 CN 200810018077 CN 200810018077 A CN200810018077 A CN 200810018077A CN 101298559 B CN101298559 B CN 101298559B
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Abstract
The invention discloses a manufacturing method of rare earth tri-phosphor mixed phosphor used for CCFL. Firstly, carry out powder slurry treatment of a water-based solution to at least two tri-phosphor rare earth phosphors obtained by a traditional physically mixing mode, and allow mixed powder to be fully mixed in the water-based solution by rapid blending; and then dilute the solution to be 3-5 times of the original powder slurry, and wash the solution with pure water for a plurality of times after screening; put dewatered powder agglomerate into a alumina crucible after drying treatment, and then carry out restoring heat treatment under the protection of inert gas at the temperature of 300-800 DEG C; finally, filter the powder agglomerate with a 100-300 mesh screen to obtain the tri-phosphor mixed phosphor powder. The method of the invention can effectively neutralize the electrical property of each component part of the mixed fluorescent powder, thus resolving the problems of mixed powder condensation and lamination occur in CCFL products, and improving the yield after pipes are manufactured with the mixed powder.
Description
Technical field
The present invention relates to a kind of preparation method of fluor, be specifically related to the preparation method of a kind of CCFL with rare earth tricolor mixing phosphor.
Background technology
CCFL (cold-cathode fluorescence lamp) is with europkium-activated many aluminate blue fluorescents body [BaMgAl10O17:Eu﹠amp with rare earth tricolor mixing phosphor; BaSrMgAl10O17:Eu], terbium activated phosphate green fluor [LaPO4:Ce, Tb], europkium-activated yttrium oxide red-emitting phosphors [Y2O3:Eu], many aluminate greens of cerium terbium activated fluor [MgAl11O19:Ce, Tb], europium manganese coactivated many aluminate blue fluorescents body [BaMgAl10O17:Eu, Mn﹠amp; BaSrMgAl10O17:Eu, Mn] and the mixture of above-mentioned two kinds or two or more fluor.
CCFL trichromatic fluorescent light tube and face are to make the powder slurry after adopting above-mentioned rareearth blue fluorescent body, rare earth green fluor, rare-earth red fluor through independent or mixing, are coated on the inner surface of tube, form fluorescent screen.In this process, traditional mixed fluorescent powder has and condenses, defectives such as layering, and there are problems such as good article rate is low in producer when using, and need carry out a large amount of sorting work.
In addition, along with the development of liquid crystal industry, the demand of CCFL becomes ascendant trend significantly, requires yield of products further to improve to reduce cost of raw materials used.Simultaneously, the rising of product good article rate can be saved the use of fluorescent material significantly; Contain your a large amount of rare earth Eu, Tb etc. in the various materials of CCFL with the rare-earth trichromatic fluor, add the restricted exploitation (exploitation) of country to rare-earth ore resource, from the aspect that economizes on resources, the preparation technology's level that improves tricolor mixing phosphor also has great social significance.
Summary of the invention
The present invention is directed to the cohesion that exists among the existing tricolor mixing phosphor preparation technology, electrically bad, problems such as layering provide a kind of improved preparation method who improves the CCFL of the good article rate behind the powder mix tubulation with rare earth tricolor mixing phosphor.
For achieving the above object, the present invention takes following technical scheme to be achieved:
A kind of CCFL is characterized in that with the manufacture method of rare earth tricolor mixing phosphor fluor, comprises the steps:
1) at first,, carries out the powder pulp of group water solution and handle, make powder mix thorough mixing in group water solution the two or more trichromatic rare-earth fluor of conventional physical hybrid mode gained;
2) will stir sufficient water base powder mix slurry adds water and is diluted to 3～5 times of original powder volume of slurry;
3) the powder mix slurry with dilution process passes through the 350-600 mesh sieve, again with pure water washing 3-5 time;
4) the powder slurry after the pure water washing is carried out processed, the powder agglomates after the dehydration is crossed 150 mesh sieves after 100-120 degree centigrade of following drying treatment;
5) powder after the drying and screening is packed into alumina crucible carries out reduction heat in 300-800 degree centigrade and handles under the protective atmosphere of rare gas element;
6) powder after the thermal treatment is crossed 100～300 mesh sieves, promptly obtain the tricolor mixing phosphor powder.
In the aforesaid method, described two or more trichromatic rare-earth fluor comprises europkium-activated many aluminate blue fluorescents body BaMgAl10O17:Eu or BaSrMgAl10O17:Eu, terbium activated phosphate green fluor LaPO4:Ce, Tb, europkium-activated yttrium oxide red-emitting phosphors Y2O3:Eu, many aluminate greens of cerium terbium activated fluor MgAl11O19:Ce, Tb, the coactivated many aluminate blue fluorescents body of europium manganese BaMgAl10O17:Eu, Mn or BaSrMgAl10O17:Eu, two or three of Mn.It is that the above-mentioned two or more powder of mentioning are placed container that the powder pulp of described group water solution is handled, and adds the pure water of its weight more than 3 times, stirs 2～5 hours with 500～800 rev/mins in stirrer, makes it become the finely starched attitude.Described rare gas element is a nitrogen.
Advantage of the present invention is, the mixed fluorescent powder that the manufacturing of conventional hybrid method is finished carries out the powder pulp to be handled, high-speed stirring can eliminate between the monochromatic powder electrically.Then powder slurry is diluted to original 3～5 times, by 300～600 order water sieves with further mixing, each component that can neutralize electrically; Mixed powder slurry carries out repeatedly the pure water washing to eliminate electrically.Through dehydrating, under the situation of protection of inert gas, carry out 300～800 degrees centigrade of calcinations and handle, can solve the monochromatic component hydrolysis problem that occurs in the water base processing.Improve the mixing phosphor that technology obtains by the present invention and can eliminate condensing of existing in the simple combination treatment of tradition, use problems such as layering efficiently solve the redness that occurs in the water base processing or the hydrolysis problem of blue emitting phophor.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
At first, europkium-activated yttrium oxide red-emitting phosphors [Y2O3:Eu] and terbium activated phosphate green fluor [LaPO4:Ce with conventional hybrid, Tb] the powder pulp of carrying out group water solution handles, be about to the above-mentioned two or more powder of mentioning and place container, add the pure water of its weight more than 3 times, in stirrer, stirred 5 hours, make it become the finely starched attitude with 500 rev/mins;
The powder slurry that stirring is finished dilutes 3 times, then by 350 eye mesh screens; With pure water washing 3 times
Powder slurry after the pure water washing is carried out processed, and the powder agglomates after the dehydration places the dry back of 100 degrees centigrade drying machine to cross 150 mesh sieves;
With the alumina crucible of packing into of the powder after the drying and screening; Carrying out reduction heat in nitrogen protection in 300 degrees centigrade handles;
Powder after the thermal treatment promptly gets product 1 by 100 mesh sieves.
Embodiment 2,
At first, with europkium-activated many aluminate blue fluorescents body [BaMgAl10O17:Eu﹠amp of conventional hybrid; BaSrMgAl10O17:Eu] and europkium-activated yttrium oxide red-emitting phosphors [Y2O3:Eu] and terbium activated phosphate green fluor [LaPO4:Ce, Tb] the powder pulp of carrying out group water solution handles, the powder pulp processing that is described group water solution is that the above-mentioned two or more powder of mentioning are placed container, add the pure water of its weight more than 3 times, in stirrer, stirred 2 hours, make it become the finely starched attitude with 800 rev/mins;
The powder slurry that stirring is finished dilutes 5 times, then by 600 eye mesh screens; With pure water washing 5 times
Powder slurry after the pure water washing is carried out processed, and the powder agglomates after the dehydration places the dry back of 120 degrees centigrade drying machine to cross 150 mesh sieves;
With the alumina crucible of packing into of the powder after the drying and screening; Carrying out reduction heat in nitrogen protection in 800 degrees centigrade handles;
Powder after the thermal treatment promptly gets product 2 by 300 mesh sieves.
Embodiment 3
At first, with europkium-activated yttrium oxide red-emitting phosphors [Y2O3:Eu], many aluminate greens of cerium terbium activated fluor [MgAl11O19:Ce, Tb], europium manganese coactivated many aluminate blue fluorescents body [BaMgAl10O17:Eu, the Mn﹠amp of conventional hybrid; BaSrMgAl10O17:Eu, Mn] carry out the powder pulp processing of group water solution, be about to the above-mentioned two or more powder of mentioning and place container, add the pure water of its weight more than 3 times, in stirrer, stirred 4 hours with 600 rev/mins, make it become the finely starched attitude;
The powder slurry that stirring is finished dilutes 4 times, then by 400 eye mesh screens; With pure water washing 4 times
Powder slurry after the pure water washing is carried out processed, and the powder agglomates after the dehydration places the dry back of 110 degrees centigrade drying machine to cross 150 mesh sieves;
With the alumina crucible of packing into of the powder after the drying and screening; Carrying out reduction heat in nitrogen protection in 600 degrees centigrade handles;
Powder after the thermal treatment promptly gets product 3 by 200 mesh sieves.
Claims (4)
1. the preparation method of a CCFL usefulness rare earth tricolor mixing phosphor is characterized in that, comprises the steps:
1) at first,, carries out the powder pulp of group water solution and handle, make powder mix thorough mixing in group water solution the two or more trichromatic rare-earth fluor of conventional physical hybrid mode gained;
2) water base powder mix slurry is added water and be diluted to 3～5 times of original powder volume of slurry;
3) the powder mix slurry with dilution process passes through the 350-600 mesh sieve, again with pure water washing 3-5 time;
4) the powder slurry after the pure water washing is carried out processed, the powder agglomates after the dehydration is crossed 150 mesh sieves after 100-120 degree centigrade of following drying treatment;
5) powder after the drying and screening is packed into alumina crucible carries out reduction heat in 300-800 degree centigrade and handles under the protective atmosphere of rare gas element;
6) powder after the thermal treatment is crossed 100～300 mesh sieves, promptly obtain the tricolor mixing phosphor powder.
2. CCFL according to claim 1 is characterized in that with the preparation method of rare earth tricolor mixing phosphor described two or more trichromatic rare-earth fluor comprise europkium-activated many aluminate blue fluorescents body BaMgAl
10O
17: Eu or BaSrMgAl
10O
17: Eu, terbium activated phosphate green fluor LaPO
4: Ce, Tb, europkium-activated yttrium oxide red-emitting phosphors Y
2O
3: Eu, many aluminate greens of cerium terbium activated fluor MgAl
11O
19: Ce, Tb, the coactivated many aluminate blue fluorescents body of europium manganese BaMgAl
10O
17: Eu, Mn or BaSrMgAl
10O
17: Eu, two or three of Mn.
3. the CCFL according to claim 1 preparation method of rare earth tricolor mixing phosphor, it is characterized in that, it is that mixed powder is placed container that the powder pulp of described group water solution is handled, add the pure water of its weight more than 3 times, in stirrer, stirred 2～5 hours, make it become the finely starched attitude with 500～800 rev/mins.
4. CCFL according to claim 1 is characterized in that with the preparation method of rare earth tricolor mixing phosphor described rare gas element is a nitrogen.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810018077 CN101298559B (en) | 2008-04-29 | 2008-04-29 | Preparation of rare earth tricolor mixing phosphor for CCFL |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200810018077 CN101298559B (en) | 2008-04-29 | 2008-04-29 | Preparation of rare earth tricolor mixing phosphor for CCFL |
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| CN101298559A CN101298559A (en) | 2008-11-05 |
| CN101298559B true CN101298559B (en) | 2010-12-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102766461A (en) * | 2012-06-29 | 2012-11-07 | 彩虹集团电子股份有限公司 | Process for improving thermal stability of lanthanum-cerium-terbium phosphate green fluorescent powder for CCFLs (cold cathode fluorescent lamps) |
| CN103113896A (en) * | 2013-01-24 | 2013-05-22 | 李迎九 | Agricultural rare earth phosphor for simulating sunshine light source |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3220286B2 (en) * | 1993-05-17 | 2001-10-22 | 高砂熱学工業株式会社 | Operating method of heat source system for environmental test room |
| CN1506438A (en) * | 2002-12-07 | 2004-06-23 | 中国科学院长春光学精密机械与物理研 | Post-treatment covering method of luminophor for color plasma plate display |
| CN1632050A (en) * | 2004-11-16 | 2005-06-29 | 彩虹集团电子股份有限公司 | Method for producing phosphor powder |
| CN1664050A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Method for post-treatment of fluorescent materials |
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2008
- 2008-04-29 CN CN 200810018077 patent/CN101298559B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3220286B2 (en) * | 1993-05-17 | 2001-10-22 | 高砂熱学工業株式会社 | Operating method of heat source system for environmental test room |
| CN1506438A (en) * | 2002-12-07 | 2004-06-23 | 中国科学院长春光学精密机械与物理研 | Post-treatment covering method of luminophor for color plasma plate display |
| CN1632050A (en) * | 2004-11-16 | 2005-06-29 | 彩虹集团电子股份有限公司 | Method for producing phosphor powder |
| CN1664050A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Method for post-treatment of fluorescent materials |
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