CN104130770A - Surface treatment method of high luminous efficiency white light LED (light-emitting diode) use orange fluorescent powder - Google Patents
Surface treatment method of high luminous efficiency white light LED (light-emitting diode) use orange fluorescent powder Download PDFInfo
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- CN104130770A CN104130770A CN201410305471.3A CN201410305471A CN104130770A CN 104130770 A CN104130770 A CN 104130770A CN 201410305471 A CN201410305471 A CN 201410305471A CN 104130770 A CN104130770 A CN 104130770A
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Abstract
A surface treatment method of high luminous efficiency white light LED (light-emitting diode) use orange fluorescent powder is as follows: first, using In2O3 for first-time surface treatment and sintering, then using nano SiO2 for secondary surface treatment, filtering by suction, drying and sieving to obtain surface treated fluorescent powder, and the surface treatment method can be used for surface treatment of synthetic silicate orange fluorescent powder, and has the characteristics of products have good luminescent properties and superior anti attenuation performance.
Description
Technical field
The present invention relates to technical field prepared by fluorescent material, particularly the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs.
Background technology
White light LEDs has energy-saving and environmental protection, green, the remarkable advantage such as efficient, as a kind of novel all solid state lighting source, is deeply subject to people's attention.In recent years, along with deepening continuously of semiconductive luminescent materials research, LED manufactured the development and application of novel process, novel material, and versicolor ultra-high brightness LED has been obtained breakthrough.The superiority such as LED illumination is high with its luminous efficiency, current consumption is few, long service life, safe reliability are strong, environmentally-friendly sanitary, are thought the mankind's one of greatest invention after Edison invented incandescent-lamp bulb by industry.
White light LEDs rare earth luminescent material is very important integral part during white light LEDs is made.In actual applications, it is main mainly containing these three kinds of yttrium aluminum garnets, silicate, nitride.Silicate series material ultraviolet, near ultraviolet and blue-light excited under, all there is higher quantum yield, its physical and chemical performance is more stable, during High-temperature Packaging not with resin reaction, be with a wide range of applications.At present, the commercial orange fluorescent material of silicate in use ubiquity luminous efficiency on the low side, in damp atmosphere, easily decompose, the shortcoming such as anti-decay property is poor.How to prepare there is high luminous efficiency, the orange fluorescent material of silicate of good moisture resistant ability, strong anti-decay property becomes the technical problem that current urgent need solves.
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 surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs, can be used in the surface treatment of synthetic silicate orange fluorescent powder, have and can prepare the orange fluorescent material of commercial LED silicate that luminescent properties is good, Deliquescence-resistant ability is strong, anti-decay property is superior.
To achieve these goals, technical scheme of the present invention is:
A surface treatment method for orange fluorescent powder for high light efficiency white light LEDs, comprises the steps:
Step 1, In
2o
3one-time surface is processed:
The orange fluorescent material of silicate is joined to the mixing solutions of indium nitrate and urea, ultrasonic dispersion 5-10min, add Surfactant CTAB, use agitator strong stirring, turn/min of 300-400, and at 80-90 ℃, be incubated 2-4h, cooling rear centrifugation, use absolute ethanol washing 3-5 time, dry 12-24 hour at 80-120 ℃;
Step 2, calcination:
The fluorescent material powder agglomates forming after dry is crossed to 100 mesh sieves, put into alumina crucible, under nitrogen atmosphere, in 600-800 ℃ of calcination 1-5 hour, fluorescent material is crossed to 100 mesh sieves after cooling, obtain surface treatment primary product;
Step 3, nanometer SiO
2secondary surface preparation:
By 5-30 quality pure water powder pulp doubly for gained surface treatment primary product in step 2, cross 500 eye mesh screens, remove screening reject, then add in mass ratio the nanometer SiO of 0.001%-0.05%
2, stir 1-2 hour, then suction filtration or dehydration, at 100-120 ℃, dry 6-24 hour, crosses 100 eye mesh screens by dried fluorescent material, can obtain the orange fluorescent powder surface process finished product of silicate for LED.
Described indium nitrate strength of fluid is 0.001mol/L-0.1mol/L.
The mass ratio of the described indium nitrate adding and silicate fluorescent powder is 0.03:1-0.05:1.
The mass ratio of the described urea adding and silicate fluorescent powder is: 0.16:1-0.26:1.
The mass ratio of the described tensio-active agent adding and silicate fluorescent powder is: 0.0045:1-0.0055:1.
In described step 2, nitrogen atmosphere refers to that nitrogen flow is 1-3 cube m/h.
Nanometer SiO in described step 3
2self-control silicon-dioxide for 10-15nm.
Because the present invention adopts unique formula, when surface treatment, adopt distinctive In
2o
3process, calcination partly adopts nitrogen atmosphere, finally adds nanometer SiO
2carry out secondary surface preparation, so produce the orange fluorescent material of commercial LED silicate that luminescent properties is good, Deliquescence-resistant ability is strong, anti-decay property is superior.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment mono-
A surface treatment method for orange fluorescent powder for high light efficiency white light LEDs, comprises the steps:
Step 1, In
2o
3one-time surface is processed:
2.0g urea is joined in the indium nitrate solution that 100ml concentration is 0.01mol/L, after mixing, add the orange fluorescent material of 10g silicate, ultrasonic dispersion 5min.Add 0.049g Surfactant CTAB, use agitator strong stirring, 350 turn/min, and be incubated 2h at 80 ℃, cooling rear centrifugation, is used absolute ethanol washing 3 times, at 100 ℃, is dried 12 hours;
Step 2, calcination:
The fluorescent material powder agglomates forming after dry is crossed to 100 mesh sieves, put into alumina crucible, under nitrogen atmosphere (nitrogen flow is 1 cube m/h), in 600 ℃ of calcinations 3 hours, fluorescent material is crossed to 100 mesh sieves after cooling, obtain surface treatment primary product;
Step 3, nanometer SiO
2secondary surface preparation:
Resulting fluorescent material in step 2 is joined in pure water, and mass ratio is 1:8, after powder pulp, crosses 500 mesh sieves, removes screening reject, adds the nanometer SiO of fluorescent material quality 0.002%
2(10nm) stir 1 hour, then suction filtration is dried 6 hours at 120 ℃, and dried fluorescent material is crossed 100 eye mesh screens, can obtain the orange fluorescent powder surface process finished product of silicate for LED.This fluorescent material initial stage brightness 100, after heat fade, brightness is 98.
Embodiment bis-
A surface treatment method for orange fluorescent powder for high light efficiency white light LEDs, comprises the steps:
Step 1, In
2o
3one-time surface is processed:
12.0g urea is joined in the indium nitrate solution that 400ml concentration is 0.02mol/L, after mixing, add the orange fluorescent material of 60g silicate, ultrasonic dispersion 5min.Add 0.3g Surfactant CTAB, use agitator strong stirring, 350 turn/min, and be incubated 1h at 100 ℃, cooling rear centrifugation, is used absolute ethanol washing 3 times, at 100 ℃, is dried 16 hours;
Step 2, calcination:
The fluorescent material powder agglomates forming after dry is crossed to 100 mesh sieves, put into alumina crucible, under nitrogen atmosphere (nitrogen flow is 1 cube m/h), in 600 ℃ of calcinations 4 hours, fluorescent material is crossed to 100 mesh sieves after cooling, obtain surface treatment primary product;
Step 3, nanometer SiO2 secondary surface preparation:
Resulting fluorescent material in step 2 is joined in pure water, mass ratio is 1:10, after powder pulp, cross 500 mesh sieves, remove screening reject, add the nanometer SiO2 (13nm) of fluorescent material quality 0.002% to stir 1 hour, then suction filtration, at 100 ℃, be dried 10 hours, dried fluorescent material is crossed 100 eye mesh screens, can obtain the orange fluorescent powder surface process finished product of silicate for LED.This fluorescent material initial stage brightness 102, after heat fade, brightness is 100.
Embodiment tri-
A surface treatment method for orange fluorescent powder for high light efficiency white light LEDs, comprises the steps:
Step 1, In2O3 one-time surface is processed:
30.0g urea is joined in the indium nitrate solution that 800ml concentration is 0.03mol/L, after mixing, add the orange fluorescent material of 150g silicate, ultrasonic dispersion 10min.Add 0.785g Surfactant CTAB, use agitator strong stirring (400 turn/min), and be incubated 4h at 80 ℃, cooling rear centrifugation, is used absolute ethanol washing 3 times, at 100 ℃, is dried 24 hours;
Step 2, calcination:
The fluorescent material powder agglomates forming after dry is crossed to 100 mesh sieves, put into alumina crucible, under nitrogen atmosphere (nitrogen flow is 2 cubes ms/h), in 700 ℃ of calcinations 3 hours, fluorescent material is crossed to 100 mesh sieves after cooling, obtain surface treatment primary product;
Step 3, nanometer SiO2 secondary surface preparation:
Resulting fluorescent material in step 2 is joined in pure water after (mass ratio is 1:23) powder pulp, cross 500 mesh sieves, remove screening reject, add the nanometer SiO2 (10nm) of fluorescent material quality 0.01% to stir 1 hour, then suction filtration, at 120 ℃, be dried 10 hours, dried fluorescent material is crossed 100 eye mesh screens, can obtain the orange fluorescent powder surface process finished product of silicate for LED.This fluorescent material initial stage brightness 100, after heat fade, brightness is 99.
Embodiment tetra-
A surface treatment method for orange fluorescent powder for high light efficiency white light LEDs, comprises the steps:
Step 1, In2O3 one-time surface is processed:
70.0g urea is joined in the indium nitrate solution that 2500ml concentration is 0.02mol/L, after mixing, add the orange fluorescent material of 300g silicate, ultrasonic dispersion 10min.Add 1.625g Surfactant CTAB, use agitator strong stirring (400 turn/min), and be incubated 3h at 80 ℃, cooling rear centrifugation, is used absolute ethanol washing 5 times, at 100 ℃, is dried 24 hours;
Step 2, calcination:
The fluorescent material powder agglomates forming after dry is crossed to 100 mesh sieves, put into alumina crucible, under nitrogen atmosphere (nitrogen flow is 2.5 cubes ms/h), in 800 ℃ of calcinations 3 hours, fluorescent material is crossed to 100 mesh sieves after cooling, obtain surface treatment primary product;
Step 3, nanometer SiO2 secondary surface preparation:
Resulting fluorescent material in step 2 is joined in pure water, mass ratio is 1:25, after powder pulp, cross 500 mesh sieves, remove screening reject, add the nanometer SiO2 (14nm) of fluorescent material quality 0.002% to stir 2 hours, then suction filtration, at 120 ℃, be dried 24 hours, dried fluorescent material is crossed 100 eye mesh screens, can obtain the orange fluorescent powder surface process finished product of silicate for LED.This fluorescent material initial stage brightness 103, after heat fade, brightness is 102.
Claims (7)
1. a surface treatment method for orange fluorescent powder for high light efficiency white light LEDs, is characterized in that, comprises the steps:
Step 1, In
2o
3one-time surface is processed:
The orange fluorescent material of silicate is joined to the mixing solutions of indium nitrate and urea, ultrasonic dispersion 5-10min, add Surfactant CTAB, use agitator strong stirring, turn/min of 300-400, and be incubated 2-4h at 80-90 ℃, cooling rear centrifugation, use absolute ethanol washing 3-5 time, at 80-120 ℃, dry 12-24 hour, prepares fluorescent material powder agglomates;
Step 2, calcination:
The fluorescent material powder agglomates forming after dry is crossed to 100 mesh sieves, put into alumina crucible, under nitrogen atmosphere, in 600-800 ℃ of calcination 1-5 hour, fluorescent material is crossed to 100 mesh sieves after cooling, obtain surface treatment primary product;
Step 3, nanometer SiO
2secondary surface preparation:
By 5-30 quality pure water powder pulp doubly for gained surface treatment primary product in step 2, cross 500 eye mesh screens, remove screening reject, then add in mass ratio the nanometer SiO of 0.001%-0.05%
2, stir 1-2 hour, then suction filtration or dehydration, at 100-120 ℃, dry 6-24 hour, crosses 100 eye mesh screens by dried fluorescent material, can obtain the orange fluorescent powder surface process finished product of silicate for LED.
2. the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs according to claim 1, is characterized in that, described indium nitrate strength of fluid is 0.001mol/L-0.1mol/L.
3. the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs according to claim 1, is characterized in that, described in the indium nitrate that adds and the mass ratio of silicate fluorescent powder be 0.03:1-0.05:1.
4. the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs according to claim 1, is characterized in that, described in the urea that adds and the mass ratio of silicate fluorescent powder be: 0.16:1-0.26:1.
5. the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs according to claim 1, is characterized in that, described in the tensio-active agent that adds and the mass ratio of silicate fluorescent powder be: 0.0045:1-0.0055:1.
6. the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs according to claim 1, is characterized in that, in described step 2, nitrogen atmosphere refers to that nitrogen flow is 1-3 cube m/h.
7. the surface treatment method of orange fluorescent powder for a kind of high light efficiency white light LEDs according to claim 1, is characterized in that the nanometer SiO in described step 3
2self-control silicon-dioxide for 10-15nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106433639A (en) * | 2016-10-13 | 2017-02-22 | 河北利福光电技术有限公司 | 315 phase orange silicate fluorescent powder and preparation method thereof |
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| CN1667081A (en) * | 2005-02-25 | 2005-09-14 | 东南大学 | Alumina coated fluorescent powder and its coating method |
| WO2009149015A2 (en) * | 2008-06-02 | 2009-12-10 | University Of Victoria Innovation And Development Corporation | Blue light emitting nanomaterials and synthesis thereof |
| CN101368093A (en) * | 2008-10-13 | 2009-02-18 | 彩虹集团电子股份有限公司 | Method of producing green fluorescent powder |
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Application publication date: 20141105 |