CN101565618B - Method for preparing red phosphor for CCFL - Google Patents
Method for preparing red phosphor for CCFL Download PDFInfo
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- CN101565618B CN101565618B CN200910022773A CN200910022773A CN101565618B CN 101565618 B CN101565618 B CN 101565618B CN 200910022773 A CN200910022773 A CN 200910022773A CN 200910022773 A CN200910022773 A CN 200910022773A CN 101565618 B CN101565618 B CN 101565618B
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Abstract
The invention relates to a method for preparing red fluorescent powder, in particular to a method for preparing red fluorescent powder for a CCFL. The prior red phosphor has the defects of poor powderdispersity, large particle cohesion, time consumption for powder slurry preparation, low tube-coating rate, unsmooth film surface after the powder slurry is coated on a light tube and obvious condens ation point in the application process and the like. The method comprises the following steps: firstly, preparing a co-deposit of yttrium oxide and europium oxide and a cosolvent; secondly, mixing materials, burning the mixture after the material mixing in an oxidizing atmosphere, cooling the mixture to the room temperature, and screening the mixture to obtain a burnt finished product of the phosphor; dispersing the phosphor finished product, and slurrying; and finally, adding nanometer aluminum oxide to the powder slurry, removing the moisture content and drying, reducing the temperature to the room temperature, and screening the mixture to obtain the red phosphor. The red fluorescent powder prepared by the method has small particle cohesion, good dispersity, excellent coating performance, smooth film surface after the powder slurry is coated on a light tube, and no obvious condensation point.
Description
One, technical field
The present invention relates to a kind of preparation method of red fluorescence powder, particularly a kind of CCFL is with the preparation method of red fluorescence powder.
Two, background technology
The type cold-cathode fluorescence lamp development of high in recent years light efficiency tubule footpath is very fast, and its used red fluorescence powder is with Y
2O
3: Eu is the substrate material red fluorescence powder.Y
2O
3: the Eu red fluorescence powder is a white powder, isometric system, and it is an effectively luminescent material under the 253.7nm burst of ultraviolel, under the 253.7nm burst of ultraviolel, sends fluorescent red-orange, peak wavelength is 611nm; Its chromaticity coordinates can change because of the difference of europium content, and general x is between 0.646～0.654, and y is between 0.346～0.351.The red fluorescence powder that is applied to tubule footpath type cold-cathode fluorescence lamp (CCFL) does not in the market have too big-difference aspect the characteristics of luminescence; Powder dispersity is poor, particle aggregation is big but exist in application facet; In application process, exist powder process slurry consuming time, be coated with that the pipe rate is not high, the powder slurry is coated in shortcomings such as face on the fluorescent tube is rough, coacervation point is obvious, brings negative impact for tubule footpath type cold-cathode fluorescence lamp light efficiency.
Three, summary of the invention
The object of the present invention is to provide the preparation method of a kind of CCFL with red fluorescence powder, the red fluorescence powder powder dispersity is poor in the traditional technology, cohesion is serious to solve, the problem of application characteristic difference.
For reaching above-mentioned technical purpose, the present invention includes following operation steps:
Get the raw materials ready:
(1) purchases the solubility promoter that contains the yttrium europium oxide codeposition body that mass percent is 5.6～9.0% europiums and cross 100 mesh sieves;
Batch mixing:
(2) getting the yttrium europium oxide codeposition body is raw material, adds the fusing assistant of yttrium europium oxide codeposition body quality 0.5%～2%, and thorough mixing obtains mixture A;
Burn till:
(3) with said mixture A calcination 3～6 hours under 1200 ℃～1500 ℃ oxidizing atmosphere, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
(4) fluor is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight being 1: 2～4: 2～4 to disperse, and disperseing rotating speed is 20～40 commentariess on classics/min, and jitter time is 1～4 hour, obtains powder and starches A;
Slurrying:
(5) the powder slurry A that obtains after will disperseing crosses 300～500 order water sieves, and burns till article by fluor: 1: 10 condition of the weight ratio of water wash more than 5 times, outwells clear liquid after the sedimentation and obtains powder and starch B; Again powder is starched B and change in 1000 liters of surface treatment grooves, burn till article by fluor: the weight ratio of ionized water=1: 2～4 adds ionized water, stirs 30min to evenly, obtains powder slurry C;
Finished product:
(6) burn till article by the 1kg fluor and add 0.025～5g nano aluminium oxide in powder slurry C, and be 60～80 commentariess on classics/min with stirring velocity, stirring 30～60min obtains mixture D;
(7) remove moisture contained in the mixture D at last, and be under 100～130 ℃ the condition dry 6～12 hours with drying temperature, temperature is sieved after reducing to room temperature, obtains red-emitting phosphors.
Above-mentioned fusing assistant is one or more in boric acid, boron oxide, bariumchloride, barium tetraborate, tetraboric acid magnesium, the Trilithium phosphate.
Advantage of the present invention is: utilize the cohesion of the made red-emitting phosphors powder granule of the present invention little, good dispersibility, coating property face excellent, that the powder slurry is coated on the fluorescent tube are smooth, do not have obvious coacervation point.
Four, embodiment
Embodiment 1:
Get the raw materials ready:
1. purchase and contain the yttrium europium oxide codeposition body and the fusing assistant of crossing 100 mesh sieves that mass percent is 5.6% europium; Described solubility promoter is boron oxide and the bariumchloride mixture by 1: 10 mixed of mass ratio.
Batch mixing:
2. getting the yttrium europium oxide codeposition body is raw material, adds the fusing assistant of yttrium europium oxide codeposition body quality 1.0%, obtains mixture A behind the thorough mixing;
Burn till:
3. with the mixture A alumina crucible of packing into, be placed in the electric continuous tunnel furnace of oxidizing atmosphere 1360 ℃ of calcinations 3 hours, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
4. red-emitting phosphors is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight being to disperse at 1: 2: 2, and disperseing rotating speed is 40 commentariess on classics/min, and jitter time is 3 hours, obtains powder and starches A;
Slurrying:
5. the powder slurry A that will obtain after will disperseing crosses 300 order water sieves, and burns till article by fluor: 1: 10 condition of the weight ratio of water washing 5 times, and outwell clear liquid after the sedimentation and obtain powder slurry B; Again powder is starched B and change in 1000 liters of surface treatment grooves, inject by weight burning till article for fluor: the ionized water of ionized water=1: 2, stir 30min to evenly, obtain powder slurry C;
Finished product:
6. burn till article by the 1kg fluor and add the 0.025g nano aluminium oxide in powder slurry C, and be 65 commentariess on classics/min with stirring velocity, stirring 30min obtains mixture D;
7. remove moisture contained in the mixture D at last, and be under 100 ℃ the condition dry 6 hours with drying temperature, temperature is crossed 100 mesh sieves after reducing to room temperature, can obtain required red-emitting phosphors sample 1.
Embodiment 2:
Get the raw materials ready:
1. purchase and contain the yttrium europium oxide codeposition body and the fusing assistant of crossing 100 mesh sieves that mass percent is 8.0% europium: boric acid;
Batch mixing:
2. getting the yttrium europium oxide codeposition body is raw material, adds the boric acid of yttrium europium oxide codeposition body quality 0.5%, obtains mixture A behind the thorough mixing;
Burn till:
3. with the mixture A alumina crucible of packing into, be placed in the electric continuous tunnel furnace of oxidizing atmosphere 1500 ℃ of calcinations 4 hours, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
4. fluor is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight being to disperse at 1: 2: 2, and disperseing rotating speed is 40 commentariess on classics/min, and jitter time is 1 hour, obtains powder and starches A;
Slurrying:
5. the powder slurry A that will obtain after will disperseing crosses 400 order water sieves, and burns till article by fluor: 1: 10 condition of the weight ratio of water washing 6 times, and outwell clear liquid after the sedimentation and obtain powder slurry B; Again powder is starched B and change in 1000 liters of surface treatment grooves, burn till article by weight fluor: ionized water=add ionized water at 1: 3, stir 30min to evenly, obtain powder slurry C;
Finished product:
6. burn till article by the 1kg fluor and add the 0.5g nano aluminium oxide in powder slurry C, and be 65 commentariess on classics/min with stirring velocity, stirring 40min obtains mixture D;
7. remove moisture contained in the mixture D at last, and be under 120 ℃ the condition dry 7 hours with drying temperature, temperature is crossed 100 mesh sieves after reducing to room temperature, can obtain required red-emitting phosphors sample 2.
Embodiment 3:
Get the raw materials ready:
1. purchase and contain the yttrium europium oxide codeposition body and the fusing assistant Trilithium phosphate of crossing 100 mesh sieves that mass percent is 7.0% europium;
Batch mixing:
2. getting the yttrium europium oxide codeposition body is raw material, and add the fusing assistant of yttrium europium oxide codeposition body quality 1.0%: Trilithium phosphate obtains mixture A behind the thorough mixing;
Burn till:
3. with the mixture A alumina crucible of packing into, be placed in the electric continuous tunnel furnace of oxidizing atmosphere 1400 ℃ of calcinations 3 hours, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
4. red-emitting phosphors is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight being to disperse at 1: 2: 3, and disperseing rotating speed is 40 commentariess on classics/min, and jitter time is 4 hours, obtains powder and starches A;
Slurrying:
5. the powder slurry A that will obtain after will disperseing crosses 400 order water sieves, and burns till article by fluor: 1: 10 condition of the weight ratio of water washing 5 times, and outwell clear liquid after the sedimentation and obtain powder slurry B; Again powder is starched B and change in 1000 liters of surface treatment grooves, burn till article by weight fluor: ionized water=add ionized water at 1: 3, stir 30min to evenly, obtain powder slurry C;
Finished product:
6. burn till article by the 1kg fluor and add the 2.0g nano aluminium oxide in powder slurry C, and be 65 commentariess on classics/min with stirring velocity, stirring 40min obtains mixture D;
7. remove moisture contained in the mixture D at last, and be under 120 ℃ the condition dry 8 hours with drying temperature, temperature is crossed 100 mesh sieves after reducing to room temperature, can obtain required red-emitting phosphors sample 3.
Embodiment 4:
Get the raw materials ready:
1. purchase and contain the yttrium europium oxide codeposition body and the solubility promoter of crossing 100 mesh sieves that mass percent is 6.0% europium: barium tetraborate;
Batch mixing:
2. getting the yttrium europium oxide codeposition body is raw material, adds the fusing assistant barium tetraborate of yttrium europium oxide codeposition body quality 1.2%, obtains mixture A behind the thorough mixing;
Burn till:
3. with the mixture A alumina crucible of packing into, be placed in the electric continuous tunnel furnace of oxidizing atmosphere 1200 ℃ of calcinations 5 hours, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
4. red-emitting phosphors is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight being to disperse at 1: 3: 4, and disperseing rotating speed is 20 commentariess on classics/min, and jitter time is 2 hours, obtains powder and starches A;
Slurrying:
5. the powder slurry A that will obtain after will disperseing crosses 400 order water sieves, and burns till article by fluor: 1: 10 condition of the weight ratio of water washing 8 times, and outwell clear liquid after the sedimentation and obtain powder slurry B; Again powder is starched B and change in 1000 liters of surface treatment grooves, burn till article by weight fluor: ionized water=add ionized water at 1: 4, stir 30min to evenly, obtain powder slurry C;
Finished product:
6. burn till article by the 1kg fluor and add the 3.0g nano aluminium oxide in powder slurry C, and be 80 commentariess on classics/min with stirring velocity, stirring 50min obtains mixture D;
7. remove moisture contained in the mixture D at last, and be under 110 ℃ the condition dry 9 hours with drying temperature, temperature is crossed 100 mesh sieves after reducing to room temperature, can obtain required red-emitting phosphors sample 4.
Embodiment 5:
Get the raw materials ready:
1. purchase and contain the yttrium europium oxide codeposition body and the solubility promoter of crossing 100 mesh sieves that mass percent is 9.0% europium: tetraboric acid magnesium;
Batch mixing:
2. getting the yttrium europium oxide codeposition body is raw material, adds the tetraboric acid magnesium of yttrium europium oxide codeposition body quality 2%, obtains mixture A behind the thorough mixing;
Burn till:
3. with the mixture A alumina crucible of packing into, be placed in the electric continuous tunnel furnace of oxidizing atmosphere 1350 ℃ of calcinations 6 hours, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
4. fluor is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight being to disperse at 1: 2: 4, and disperseing rotating speed is 35 commentariess on classics/min, and jitter time is 4 hours, obtains powder and starches A;
Slurrying:
5. the powder slurry A that will obtain after will disperseing crosses 500 order water sieves, and burns till article by fluor: 1: 10 condition of the weight ratio of water washing 10 times, and outwell clear liquid after the sedimentation and obtain powder slurry B; Again powder is starched B and change in 1000 liters of surface treatment grooves, burn till article by weight fluor: ionized water=add ionized water at 1: 3, stir 30min to evenly, obtain powder slurry C;
Finished product:
6. burn till article by the 1kg fluor and add the 5.0g nano aluminium oxide in powder slurry C, and be 60 commentariess on classics/min with stirring velocity, stirring 60min obtains mixture D;
7. remove moisture contained in the mixture D at last, and be under 130 ℃ the condition dry 12 hours with drying temperature, temperature is crossed 100 mesh sieves after reducing to room temperature, can obtain required red-emitting phosphors sample 5.
Through contrasting the red fluorescence powder sample (sample 1～5) that above-mentioned 5 embodiment draw and being applied to the performance perameter between the CCFL red fluorescence powder (with reference to sample) in the market, obtain table 1:
Table 1
| Lot number | Chromaticity coordinates (x) | Chromaticity coordinates (y) | dn-ds(μm) |
| With reference to sample | 0.649 | 0.349 | 2.0 |
| Sample 1 | 0.647 | 0.350 | 0.3 |
| Sample 2 | 0.652 | 0.347 | 0.2 |
| Sample 3 | 0.651 | 0.348 | 0.1 |
| Sample 4 | 0.648 | 0.350 | 0.3 |
| Sample 5 | 0.654 | 0.346 | 0.1 |
Through last table; We can find out; What dn-ds (μ m) value reflected is powder granule cohesion characteristic; It is more little that dn-ds (μ m) is worth the cohesion between the bright powder granule of novel more, and the more little fluorescent material powder dispersity of explaining so of the cohesion between the particle is good, when the powder that makes slurry applies fluorescent tube, will be coated with that the pipe rate is high, face is smooth, coacervation point is not obvious.
Claims (2)
1. a CCFL is with the preparation method of red-emitting phosphors, and it is characterized in that: this method comprises following operation steps:
Get the raw materials ready:
(1) purchases the fusing assistant that contains the yttrium europium oxide codeposition body that mass percent is 5.6～9.0% europiums and cross 100 mesh sieves;
Batch mixing:
(2) getting the yttrium europium oxide codeposition body is raw material, adds the fusing assistant of yttrium europium oxide codeposition body quality 0.5%～2%, and thorough mixing obtains mixture A;
Burn till:
(3) with said mixture A calcination 3～6 hours under 1200 ℃～1500 ℃ oxidizing atmosphere, be cooled to room temperature then, cross 100 order dry screens, obtain fluor and burn till article;
Disperse:
(4) fluor is burnt till the article dispersion machine of packing into, and disperse by following condition, fluor burns till article: ball: water is by weight for 1:2～4:2～4 disperse, and disperseing rotating speed is 20～40 commentariess on classics/min, and jitter time is 1～4 hour, obtains powder and starches A;
Slurrying:
(5) the powder slurry A that obtains after will disperseing crosses 300～500 order water sieves, and burns till article by fluor: the condition washing of the weight ratio 1:10 of water is outwelled clear liquid and is obtained powder slurry B more than 5 times after the sedimentation; Again powder is starched B and change in 1000 liters of surface treatment grooves, burn till article by fluor: the weight ratio of ionized water=1:2～4 adds ionized water, stirs 30min to evenly, obtains powder slurry C;
Finished product:
(6) burn till article by the 1kg fluor and add 0.025～5g nano aluminium oxide in powder slurry C, and be 60～80 commentariess on classics/min with stirring velocity, stirring 30～60min obtains mixture D;
(7) remove moisture contained in the mixture D at last, and be under 100～130 ℃ the condition dry 6～12 hours with drying temperature, temperature is sieved after reducing to room temperature, obtains red-emitting phosphors.
2. a kind of CCFL according to claim 1 is characterized in that with the preparation method of red-emitting phosphors: said fusing assistant is one or more in boric acid, boron oxide, bariumchloride, barium tetraborate, tetraboric acid magnesium, the Trilithium phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910022773A CN101565618B (en) | 2009-06-01 | 2009-06-01 | Method for preparing red phosphor for CCFL |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910022773A CN101565618B (en) | 2009-06-01 | 2009-06-01 | Method for preparing red phosphor for CCFL |
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| CN101565618B true CN101565618B (en) | 2012-10-10 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101984016B (en) * | 2010-10-27 | 2013-01-16 | 彩虹集团电子股份有限公司 | Manufacturing method of red fluorescent powder used for cold cathode fluorescent lamp (CCFL) |
| CN102337129A (en) * | 2011-07-22 | 2012-02-01 | 彩虹集团电子股份有限公司 | Red luminescent fluorescent powder for FED (Field Emission Display) and preparation method thereof |
| CN102766457A (en) * | 2012-06-29 | 2012-11-07 | 彩虹集团电子股份有限公司 | Preparation method for yttrium gadolinium europium oxide red fluorescent powder applicable to 3D PDP |
| CN103305223A (en) * | 2012-09-07 | 2013-09-18 | 彩虹集团电子股份有限公司 | Manufacturing method of red fluorescent powder for tri-phosphor energy saving lamp |
| 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 |
| CN103102882A (en) * | 2013-02-28 | 2013-05-15 | 福建省长汀金龙稀土有限公司 | Preparation method of lamp rare earth three-basic-color red phosphor powder |
| CN103305209A (en) * | 2013-04-13 | 2013-09-18 | 兰州大学 | Fluxing agent for preparing Y2O3:Eu red phosphor |
| 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 |
| CN105315995B (en) * | 2015-12-03 | 2017-08-04 | 河北利福光电技术有限公司 | A kind of fluxing agent and method for preparing YAG fluorescent powder |
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| CN1664050A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Method for post-treatment of fluorescent materials |
| CN1693419A (en) * | 2005-05-23 | 2005-11-09 | 彩虹集团电子股份有限公司 | Process for preparing cathode ray luminescent material |
| CN101434837A (en) * | 2008-12-09 | 2009-05-20 | 彩虹集团电子股份有限公司 | Ultraviolet excitated red fluorescent powder surface treating method |
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- 2009-06-01 CN CN200910022773A patent/CN101565618B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664050A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Method for post-treatment of fluorescent materials |
| CN1693419A (en) * | 2005-05-23 | 2005-11-09 | 彩虹集团电子股份有限公司 | Process for preparing cathode ray luminescent material |
| CN101434837A (en) * | 2008-12-09 | 2009-05-20 | 彩虹集团电子股份有限公司 | Ultraviolet excitated red fluorescent powder surface treating method |
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