CN103351862A - Yellow fluorescent powder for white LED (Light-Emitting Diode) with high photosynthetic efficiency white and preparation method of yellow fluorescent powder - Google Patents
Yellow fluorescent powder for white LED (Light-Emitting Diode) with high photosynthetic efficiency white and preparation method of yellow fluorescent powder Download PDFInfo
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Abstract
The invention discloses yellow fluorescent powder for white LED (Light-Emitting Diode) with high photosynthetic efficiency and a preparation method of the yellow fluorescent powder. The chemical composition of the fluorescent powder is Y(3-x)Al5O12:Cex, wherein x is not smaller than 0.01 and not larger than 0.06; the preparation method of the yellow fluorescent powder comprises the following steps of: preparing a high-activity aluminum source by using aluminum nitrate as the raw material, using ammonia water as a precipitator and using polyethylene glycol as a dispersing agent; adding yttrium nitrate and cerous nitrate into the high-activity aluminum source to form a precursor solution; and drying and then pre-burning in a nitrogen gas atmosphere; and firing in a reductive atmosphere by using aluminum fluoride as a fluxing agent to obtain the yellow fluorescent powder for the white LED with high photosynthetic efficiency. And the YGA fluorescent powder which is prepared by the preparation method disclosed by the invention is regular in particle feature, uniform in particle diameter distribution, controllable in particle diameter size and capable of obtaining high light-emitting efficiency and can be used for packaging white LEDs with different requirements.
Description
Technical field
The present invention relates to the rare earth luminescent material preparing technical field, particularly a kind of yellow fluorescent powder for high light efficiency white light LEDs and preparation method thereof.
Background technology
White light LEDs namely produces the photodiode of white light emission, it is with energy-saving and environmental protection, green, the remarkable advantage such as efficient, become after incandescent light, all kinds of luminescent lamp and high-intensity gas discharge lamp the 4th generation lighting source, the every field in society is widely applied.The implementation of white light LEDs is diversified, the main implementation that adopts the blue led chip and can be combined by the yellow fluorescent powder that blue light effectively excites in present practical application, wherein, a large amount of yellow fluorescent powders that use are mainly the yttrium aluminum garnet system that cerium excites, i.e. Y
3-xAl
5O
12: Ce
x(YAG).
In the encapsulation process of white light LEDs, to be coated with at chip the mixture of one deck YAG fluorescent material and Resin adhesive, this has just proposed certain requirement to pattern and the size of fluorescent material, pattern rule, when filming, has high tap density near spherical, uniform fluorescent material, can reduce scattering of light, form easily thin and fine and close membranaceously, be conducive to obtain the white light LEDs of high light efficiency.At present, commercial YAG fluorescent material normal operation high temperature solid-state method is made, and the prepared fluorescent powder grain of this method is large, pattern is irregular, and size of particles is inhomogeneous, needs during use further to grind, and very easily introduces impurity, and causes light decay.Therefore, how to prepare the pattern rule, become the technical problem that current urgent need solves near spherical, uniform YAG fluorescent material.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of yellow fluorescent powder for high light efficiency white light LEDs and preparation method thereof, can prepare the YAG yellow fluorescent powder of granule-morphology rule, even particle size distribution, have the advantages that gained yellow fluorescent powder size is controlled, luminous efficiency is high.
In order to achieve the above object, the technical scheme taked of the present invention is:
A kind of yellow fluorescent powder for high light efficiency white light LEDs, its chemical constitution molecular formula is: Y
3-xAl
5O
12: Ce
x, 0.01≤x≤0.06 wherein.
A kind of preparation method of the yellow fluorescent powder for high light efficiency white light LEDs, its step is as follows:
Step 1: aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.01mol/L-2mol/L, polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, add-on is the 2-5% of aluminum nitrate quality, turn 90/stir 10-30min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.01mol/L-1mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until pH value stops titration when reaching 8.5-9.5, and stirring velocity is transferred to 60 turns/min, with gained mixing solutions at room temperature aging 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate and cerous nitrate, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 80-120 ℃, and the time is 12-48 hour;
Step 3: after above-mentioned steps 2 dry good presomas taking-up grindings, in nitrogen atmosphere, temperature is 500-800 ℃ of lower pre-burning 6-10 hour, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the aluminum fluoride of powder quality 0.5-2% as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Be 95:5-75:25, temperature is 1300-1500 ℃ of lower sintering 6-10 hour, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
The preparation method of the yellow fluorescent powder that is used for high light efficiency white light LEDs that the present invention adopts, the YAG fluorescent powder grain pattern rule of preparation is the almost spherical pattern, has higher tap density in packaging process of white LED, can obtain higher luminous efficiency; YAG fluorescent material particle diameter by the present invention's preparation is evenly distributed, and settling velocity is even in colloid, is easy to form thin and fine and close rete, is conducive to encapsulation; YAG fluorescent material particle diameter size by the present invention's preparation can be controlled, and can be used for the different white-light LED encapsulations that require.
Description of drawings
Fig. 1 is the Y that the present invention prepares
2.99Al
5O
12: Ce
0.01The scanning electron microscopic observation figure of yellow fluorescent powder.
Fig. 2 is the Y that the present invention prepares
2.97Al
5O
12: Ce
0.03The scanning electron microscopic observation figure of yellow fluorescent powder.
Fig. 3 is the Y that the present invention prepares
2.95Al
5O
12: Ce
0.05The scanning electron microscopic observation figure of yellow fluorescent powder.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment one:
The chemical constitution molecular formula of present embodiment fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.01 wherein.
Preparation method's step of present embodiment is as follows:
Step 1: the 313g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.05mol/L, 7g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 15min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.03mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 9.0 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 191g and cerous nitrate 0.72g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 80 ℃, and the time is 12 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 600 ℃ of lower pre-burnings 12 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 0.6g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Blending ratio is 95:5, and temperature is 1400 ℃ of lower sintering 6 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
Embodiment two:
The chemical constitution molecular formula of present embodiment fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.03 wherein.
Preparation method's step of present embodiment is as follows:
Step 1: the 938g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.07mol/L, 20g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 15min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.05mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 8.5 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 569g and cerous nitrate 6.51g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 100 ℃, and the time is 12 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 750 ℃ of lower pre-burnings 8 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 4g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Be 75:25, temperature is 1450 ℃ of lower sintering 7 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
Embodiment three:
The chemical constitution molecular formula of present embodiment fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.05 wherein.
Preparation method's step of present embodiment is as follows:
Step 1: the 187g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.01mol/L, 4g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 10min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.35mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 9.5 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 113g and cerous nitrate 2.17g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 110 ℃, and the time is 12 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 650 ℃ of lower pre-burnings 8 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 0.6g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Be 90:10, temperature is 1400 ℃ of lower sintering 6 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
Embodiment four:
The chemical constitution molecular formula of present embodiment fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.05 wherein.
Preparation method's step of present embodiment is as follows:
Step 1: the 1876g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.05mol/L, 80g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 30min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.9mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 8.9 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 1130g and cerous nitrate 21.71g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 120 ℃, and the time is 24 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 700 ℃ of lower pre-burnings 10 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 11g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Blending ratio is 80:20, and temperature is 1500 ℃ of lower sintering 8 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
Claims (9)
1. a yellow fluorescent powder that is used for high light efficiency white light LEDs is characterized in that its chemical constitution molecular formula is: Y
3-xAl
5O
12: Ce
x, 0.01≤x≤0.06 wherein.
2. a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 1 is characterized in that, the chemical constitution molecular formula of fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.01 wherein.
3. a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 1 is characterized in that, the chemical constitution molecular formula of fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.03 wherein.
4. a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 1 is characterized in that, the chemical constitution molecular formula of fluorescent material is: Y
3-xAl
5O
12: Ce
x, x=0.05 wherein.
5. the preparation method of the yellow fluorescent powder for high light efficiency white light LEDs according to claim 1 is characterized in that step is as follows:
Step 1: aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.01mol/L-2mol/L, polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, add-on is the 2-5% of aluminum nitrate quality, turn 90/stir 10-30min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.01mol/L-1mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until pH value stops titration when reaching 8.5-9.5, and stirring velocity is transferred to 60 turns/min, with gained mixing solutions at room temperature aging 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate and cerous nitrate, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 80-120 ℃, and the time is 12-48 hour;
Step 3: after above-mentioned steps 2 dry good presomas taking-up grindings, in nitrogen atmosphere, temperature is 500-800 ℃ of lower pre-burning 6-10 hour, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the aluminum fluoride of powder quality 0.5-2% as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Be 95:5-75:25, temperature is 1300-1500 ℃ of lower sintering 6-10 hour, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
6. the preparation method of a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 5 is characterized in that step is as follows:
Step 1: the 313g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.05mol/L, 7g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 15min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.03mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 9.0 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 191g and cerous nitrate 0.72g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 80 ℃, and the time is 12 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 600 ℃ of lower pre-burnings 12 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 0.6g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Blending ratio is 95:5, and temperature is 1400 ℃ of lower sintering 6 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
7. the preparation method of a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 5 is characterized in that step is as follows:
Step 1: the 938g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.07mol/L, 20g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 15min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.05mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 8.5 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 569g and cerous nitrate 6.51g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 100 ℃, and the time is 12 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 750 ℃ of lower pre-burnings 8 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 4g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Be 75:25, temperature is 1450 ℃ of lower sintering 7 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
8. the preparation method of a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 5 is characterized in that step is as follows:
Step 1: the 187g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.01mol/L, 4g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 10min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.35mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 9.5 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 113g and cerous nitrate 2.17g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 110 ℃, and the time is 12 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 650 ℃ of lower pre-burnings 8 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 0.6g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Be 90:10, temperature is 1400 ℃ of lower sintering 6 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
9. the preparation method of a kind of yellow fluorescent powder for high light efficiency white light LEDs according to claim 5 is characterized in that step is as follows:
Step 1: the 1876g aluminum nitrate is dissolved in the deionized water, be mixed with the aluminum nitrate solution that volumetric molar concentration is 0.05mol/L, 80g polyoxyethylene glycol (PEG2000) is added wherein as dispersion agent, turn 90/stir 30min under the rotating speed of min, in 50 ℃ water-bath, be that the ammoniacal liquor of 0.9mol/L carries out titration with volumetric molar concentration, simultaneously stirring velocity being adjusted into 140 turns/min, until reaching at 8.9 o'clock, pH value stops titration, and stirring velocity is transferred to 60 turns/min, the gained mixing solutions was at room temperature worn out 1 hour, prepare high reactivity aluminium source solution;
Step 2: the molar ratio by Y, Al, Ce takes by weighing respectively Yttrium trinitrate 1130g and cerous nitrate 21.71g, join in the above-mentioned steps 1 gained high reactivity aluminium source solution, with 90 turn/after the rotating speed of min stirs 2 hours, put into the baking oven inner drying, drying temperature is 120 ℃, and the time is 24 hours;
Step 3: above-mentioned steps 2 dry good presomas are taken out grinding, and in nitrogen atmosphere, temperature is 700 ℃ of lower pre-burnings 10 hours, obtains the pre-burning powder;
Step 4: after the pre-burning powder that above-mentioned steps 3 is obtained takes out and grinds, add the 11g aluminum fluoride as fusing assistant, in the mixed gas of nitrogen and hydrogen, N
2: H
2Blending ratio is 80:20, and temperature is 1500 ℃ of lower sintering 8 hours, can obtain the yellow fluorescent powder for high light efficiency white light LEDs.
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Application publication date: 20131016 |