CN103102882A - Preparation method of lamp rare earth three-basic-color red phosphor powder - Google Patents
Preparation method of lamp rare earth three-basic-color red phosphor powder Download PDFInfo
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- CN103102882A CN103102882A CN 201310063371 CN201310063371A CN103102882A CN 103102882 A CN103102882 A CN 103102882A CN 201310063371 CN201310063371 CN 201310063371 CN 201310063371 A CN201310063371 A CN 201310063371A CN 103102882 A CN103102882 A CN 103102882A
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Abstract
The invention relates to a preparation method of lamp rare earth three-basic-color red phosphor powder. The component of the lamp rare earth three-basic-color red phosphor powder is Y2O3:Eu<3+>. The preparation method comprises the following steps of: selecting appropriate yttrium europium oxide, cooperating an appropriate proportion of fluxing agent, fully mixing, sintering by virtue of an oxidizing atmosphere furnace, controlling the granularity by virtue of a ball grinding mill by utilizing a wet grinding manner, and then washing, spin-drying and drying to obtain the rare earth three-basic-color red phosphor red powder. By utilizing the preparation method, the use ratio of the powder in a lamp is effectively improved, the use amount of the red powder in the lamp is reduced, the glowing effect is ensured simultaneously, and the red powder has good dispersibility and coating properties.
Description
Technical field
The present invention relates to a kind of preparation method of red fluorescence powder, particularly a kind of straight pipe type electricity-saving lamp preparation method of rare-earth trichromatic red fluorescence powder.
Background technology
In recent years, energy-conservation requirement is more and more higher, and the straight pipe type fluorescent lamp development of high light efficiency, high loading is very fast, and its red fluorescence powder used is Y
2O
3: Eu
3+Red fluorescence powder for substrate material.Y
2O
3: Eu
3Red fluorescence powder is white powder, and isometric system under the 253.7nm ultraviolet excitation, sends efficient red fluorescence, and peak wavelength is 611nm.Traditional lamp phosphor powder utilization ratio is lower, and coating property is obviously not enough.
Summary of the invention
The objective of the invention is to be to provide a kind of straight pipe type lamp phosphor material preparation method, solved its coating property of traditional red fluorescence powder not enough, use poor problem.
1. material choice
Containing massfraction is the coprecipitated thing of yttrium europium oxide of 4.6 ~ 7.5% europiums, 99.99% yttrium oxide, 99.9% europium sesquioxide and the solubility promoter of crossing 65 mesh sieves;
2. mix
Getting the coprecipitated thing of yttrium europium oxide, yttrium oxide or europium sesquioxide is main raw material, adds 0.4% ~ 3.5% auxiliary agent of main raw material quality, fully mixes, and obtains mixture R1;
3. burn till
Mixture R1 is placed in the atmosphere furnace of 1150 ~ 1450 ℃ calcination 1 ~ 5 hour, and is cooled to room temperature, cross 10 order horizontal screens, by the time burn till product R2;
4. Ball milling
To burn till product R2 adds appropriate high purity water to carry out slurry, obtain slurry R3, slurry R3 is injected ball-milling dispersion machine, and carry out Ball milling by following condition, burn till product: abrading-ball: high purity water carries out Ball milling for 1:1 ~ 2:1 ~ 3 in mass ratio, the ball-milling dispersion machine rotating speed is 1 ~ 10 to turn/min, and the Ball milling time is 4 ~ 14 hours, obtains powder slurry R4;
5. clean, dewater
Powder is starched R4 cross 10 ~ 300 order water sieves, and inject rinse bath by burning till product: the condition warm water of the mass ratio 1:8 of high purity water cleans 2 ~ 6 times, and annotates warm water at every turn and clean stirring after 5 ~ 30 minutes, crosses 400 ~ 600 mesh sieves after the supernatant liquor of draining after sedimentation, sloughs moisture;
6. dry, finished product screen
At last the powder after dehydration was packed in the dryer of 100 ~ 500 ℃ dry 2 ~ 20 hours, temperature is down to room temperature, crosses 100 ~ 200 mesh sieves, obtains red-emitting phosphors.
Above-mentioned solubility promoter is one or several of boric acid, bariumchloride, barium chloride, barium fluoride, lithium fluoride, ammonium chloride kind.
Advantage of the present invention is: with the red-emitting phosphors excellent property of the present invention's preparation, and on lamp processed uses, good dispersity, coating property is good, and the general red fluorescence powder of dusting amount ratio is saved.
Embodiment
Example 1
1. material choice
Containing massfraction is the coprecipitated thing of yttrium europium oxide of 4.6% europium and the solubility promoter of crossing 65 mesh sieves;
2. mix
Getting the coprecipitated thing of yttrium europium oxide is main raw material, adds the mass ratio 1:0.3 of above-mentioned auxiliary agent barium chloride and boric acid, fully mixes, and obtains mixture R1;
3. burn till
Mixture R1 is packed in corundum crucible, be placed in the atmosphere furnace of 1400 ℃ calcination 1 hour, and be cooled to room temperature, cross 10 order horizontal screens, by the time burn till product R2;
4. Ball milling
To burn till product R2 adds high purity water to stir slurry, obtain slurry R3, slurry R3 is injected ball-milling dispersion machine, and carry out Ball milling by following condition, burn till product: abrading-ball: high purity water carries out Ball milling for 1:1:1 in mass ratio, the ball-milling dispersion machine rotating speed is 10 to turn/min, and the Ball milling time is 6 hours, obtains powder slurry R4;
5. clean, dewater
Powder is starched R4 cross 200 order water sieves, and inject rinse bath by burning till product: the condition warm water of the mass ratio 1:8 of high purity water cleans 2 times, and annotates warm water at every turn and clean stirring after 20 minutes, crosses 400 mesh sieves after the supernatant liquor of draining after sedimentation, sloughs moisture;
6. dry, finished product screen
At last the powder after dehydration was packed in the dryer of 120 ℃ dry 10 hours, temperature is down to room temperature, crosses 150 mesh sieves, obtains red-emitting phosphors.
Example 2
1. material choice
The solubility promoter of yttrium oxide, europium sesquioxide and mistake 65 mesh sieves;
2. mix
Yttrium oxide or europium sesquioxide (by 6.6% preparation of total amount) are main raw material, add the mass ratio 1:0.3:0.24 of above-mentioned auxiliary agent boric acid, barium fluoride and ammonium chloride fully to mix, and obtain mixture R1;
3. burn till
Mixture R1 is packed in corundum crucible, be placed in the atmosphere furnace of 1380 ℃ calcination 2 hours, and be cooled to room temperature, cross 10 order horizontal screens, by the time burn till product R2;
4. Ball milling
To burn till product R2 adds high purity water to stir slurry, obtain slurry R3, slurry R3 is injected ball-milling dispersion machine, and carry out Ball milling by following condition, burn till product: abrading-ball: high purity water carries out Ball milling for 1:1.05:1.5 in mass ratio, the ball-milling dispersion machine rotating speed is 7 to turn/min, and the Ball milling time is 10 hours, obtains powder slurry R4;
5. clean, dewater
Powder is starched R4 cross 200 order water sieves, and inject rinse bath by burning till product: the condition warm water of the mass ratio 1:10 of high purity water cleans 6 times, and annotates warm water at every turn and clean stirring after 30 minutes, crosses 400 mesh sieves after the supernatant liquor of draining after sedimentation, sloughs moisture;
6. dry, finished product screen
At last the powder after dehydration was packed in the dryer of 150 ℃ dry 16 hours, temperature is down to room temperature, crosses 150 mesh sieves, obtains red-emitting phosphors.
Example 3
1. material choice
Containing massfraction is the coprecipitated thing of yttrium europium oxide of 5.8% europium and the solubility promoter of crossing 65 mesh sieves;
2. mix
Get the coprecipitated thing of yttrium europium oxide (the europium massfraction is 6.6%), yttrium oxide is main raw material, adds the mass ratio 1:0.03 of above-mentioned auxiliary agent barium chloride and boric acid, fully mixes, and obtains mixture R1;
3. burn till
Mixture R1 is packed in corundum crucible, be placed in the atmosphere furnace of 1450 ℃ calcination 2 hours, and be cooled to room temperature, cross 10 order horizontal screens, by the time burn till product R2;
4. Ball milling
To burn till product R2 adds high purity water to stir slurry, obtain slurry R3, slurry R3 is injected ball-milling dispersion machine, and carry out Ball milling by following condition, burn till product: abrading-ball: high purity water carries out Ball milling for 1:2:3 in mass ratio, the ball-milling dispersion machine rotating speed is 7 to turn/min, and the Ball milling time is 14 hours, obtains powder slurry R4;
5. clean, dewater
Powder is starched R4 cross 200 order water sieves, and inject rinse bath by burning till product: the condition warm water of the mass ratio 1:9 of high purity water cleans 4 times, and annotates warm water at every turn and clean stirring after 10 minutes, crosses 400 mesh sieves after the supernatant liquor of draining after sedimentation, sloughs moisture;
6. dry, finished product screen
At last the powder after dehydration was packed in the dryer of 250 ℃ dry 6 hours, temperature is down to room temperature, crosses 150 mesh sieves, obtains red-emitting phosphors.
Example 4
1. material choice
Containing massfraction is the coprecipitated thing of yttrium europium oxide of 7.5% europium and the solubility promoter of crossing 65 mesh sieves;
2. mix
Getting the coprecipitated thing of yttrium europium oxide is main raw material, adds the mass ratio 1:8:1.2 of above-mentioned auxiliary agent boric acid, bariumchloride and ammonium chloride, fully mixes, and obtains mixture R1;
3. burn till
Mixture R1 is packed in corundum crucible, be placed in the atmosphere furnace of 1250 ℃ calcination 1 hour, and be cooled to room temperature, cross 10 order horizontal screens, by the time burn till product R2;
4. Ball milling
To burn till product R2 adds high purity water to stir slurry, obtain slurry R3, slurry R3 is injected ball-milling dispersion machine, and carry out Ball milling by following condition, burn till product: abrading-ball: high purity water carries out Ball milling for 1:1.7:2 in mass ratio, the ball-milling dispersion machine rotating speed is 10 to turn/min, and the Ball milling time is 6 hours, obtains powder slurry R4;
5. clean, dewater
Powder is starched R4 cross 150 order water sieves, and inject rinse bath by burning till product: the condition warm water of the mass ratio 1:10 of high purity water cleans 5 times, and annotates warm water at every turn and clean stirring after 30 minutes, crosses 400 mesh sieves after the supernatant liquor of draining after sedimentation, sloughs moisture;
6. dry, finished product screen
At last the powder after dehydration was packed in the dryer of 180 ℃ dry 18 hours, temperature is down to room temperature, crosses 150 mesh sieves, obtains red-emitting phosphors.
Claims (2)
1. a lamp with the preparation method of rare-earth trichromatic red fluorescence powder, is characterized in that:
1. material choice
Containing massfraction is the coprecipitated thing of yttrium europium oxide of 4.6 ~ 7.5% europiums, 99.99% yttrium oxide, 99.9% europium sesquioxide and the solubility promoter of crossing 65 mesh sieves;
2. mix
Getting the coprecipitated thing of yttrium europium oxide, yttrium oxide or europium sesquioxide is main raw material, adds 0.4% ~ 3.5% auxiliary agent of main raw material quality, fully mixes, and obtains mixture R1;
3. burn till
Mixture R1 is placed in the atmosphere furnace of 1150 ~ 1450 ℃ calcination 1 ~ 5 hour, and is cooled to room temperature, cross 10 order horizontal screens, by the time burn till product R2;
4. Ball milling
To burn till product R2 adds appropriate high purity water to carry out slurry, obtain slurry R3, slurry R3 is injected ball-milling dispersion machine, and carry out Ball milling by following condition, burn till product: abrading-ball: high purity water carries out Ball milling for 1:1 ~ 2:1 ~ 3 in mass ratio, the ball-milling dispersion machine rotating speed is 1 ~ 10 to turn/min, and the Ball milling time is 4 ~ 14 hours, obtains powder slurry R4;
5. clean, dewater
Powder is starched R4 cross 10 ~ 300 order water sieves, and inject rinse bath by burning till product: the condition warm water of the mass ratio 1:8 of high purity water cleans 2 ~ 6 times, and annotates warm water at every turn and clean stirring after 5 ~ 30 minutes, crosses 400 ~ 600 mesh sieves after the supernatant liquor of draining after sedimentation, sloughs moisture;
6. dry, finished product screen
At last the powder after dehydration was packed in the dryer of 100 ~ 500 ℃ dry 2 ~ 20 hours, temperature is down to room temperature, crosses 100 ~ 200 mesh sieves, obtains red-emitting phosphors.
2. a kind of lamp as claimed in claim 1 with the preparation method of rare-earth trichromatic red fluorescence powder, is characterized in that: above-mentioned solubility promoter is one or several of boric acid, bariumchloride, barium chloride, barium fluoride, lithium fluoride, ammonium chloride kind.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310063371 CN103102882A (en) | 2013-02-28 | 2013-02-28 | Preparation method of lamp rare earth three-basic-color red phosphor powder |
| CN2013101400539A CN103275714A (en) | 2013-02-28 | 2013-04-22 | Preparation method for rare earth tricolored red phosphor used for lamp |
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| CN 201310063371 CN103102882A (en) | 2013-02-28 | 2013-02-28 | Preparation method of lamp rare earth three-basic-color red phosphor powder |
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| CN 201310063371 Pending CN103102882A (en) | 2013-02-28 | 2013-02-28 | Preparation method of lamp rare earth three-basic-color red phosphor powder |
| CN2013101400539A Pending CN103275714A (en) | 2013-02-28 | 2013-04-22 | Preparation method for rare earth tricolored red phosphor used for lamp |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589428A (en) * | 2013-12-06 | 2014-02-19 | 九江有色金属冶炼有限公司 | Preparation method of rare earth red fluorescent powder of bulb for high-temperature-resistant lamp and product prepared therethrough |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100932978B1 (en) * | 2007-11-28 | 2009-12-21 | 삼성에스디아이 주식회사 | White phosphor, light emitting device using the same, and liquid crystal display using the light emitting device as a backlight unit |
| KR100898288B1 (en) * | 2008-01-09 | 2009-05-18 | 삼성에스디아이 주식회사 | White phosphor, light emission device with the same, and liquid crsytal display device with the light emission device as back light unit |
| CN101565618B (en) * | 2009-06-01 | 2012-10-10 | 彩虹集团电子股份有限公司 | Method for preparing red phosphor for CCFL |
| CN101974333B (en) * | 2010-10-22 | 2013-05-08 | 彩虹集团电子股份有限公司 | Method for manufacturing fine red fluorescent powder |
| CN102888223A (en) * | 2012-09-07 | 2013-01-23 | 彩虹集团电子股份有限公司 | Manufacture method for red fluorescent powder for three-primary-color energy saving lamp |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589428A (en) * | 2013-12-06 | 2014-02-19 | 九江有色金属冶炼有限公司 | Preparation method of rare earth red fluorescent powder of bulb for high-temperature-resistant lamp and product prepared therethrough |
| CN103589428B (en) * | 2013-12-06 | 2015-11-25 | 九江有色金属冶炼有限公司 | A kind of high temperature resistant lamp ball bubble preparation method of rare earth red fluorescent powder and the product of preparation thereof |
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| CN103275714A (en) | 2013-09-04 |
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Application publication date: 20130515 |