CN102994090A - Preparation and application of orange-yellow fluorescent powder for light-emitting diode - Google Patents

Preparation and application of orange-yellow fluorescent powder for light-emitting diode Download PDF

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CN102994090A
CN102994090A CN 201210574859 CN201210574859A CN102994090A CN 102994090 A CN102994090 A CN 102994090A CN 201210574859 CN201210574859 CN 201210574859 CN 201210574859 A CN201210574859 A CN 201210574859A CN 102994090 A CN102994090 A CN 102994090A
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sintering
light
preparation
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fluorescent powder
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王凤兰
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Abstract

The invention relates to preparation and application of orange-yellow fluorescent powder for a light-emitting diode. The chemical formula of the fluorescent powder is (Y(3-x-y), Rx)Al5O12-k/2Fk:Cey, wherein R is one or more of Ba, Gd and Tb; F-ion is introduced byfluoride, the cation is one or two of Ba and Al, wherein x is not smaller than 0.05 and not bigger than 0.2, y is not smaller than 0.05 and not bigger than 0.4, and k is not smaller than 0.3 and not bigger than 1.2. Oxide or hydroxide in the structural formula is selected, placed to a corundum crucible after being ball-milled for 24 hours, put to a box type atmosphere furnace for calcinations, cooled and sieved to obtain orange-yellow fluorescent powder which can be effectively aroused by ultraviolet light and blue light to emit an orange-yellow light spectrum with peak wavelength of 570 nanometers to 580 nanometers, and dominant wavelength of 580 nanometers to 590 nanometers, can be directly applied to a warm-white LED (Light-Emitting Diode) product, or can be combined with traditional YAG (Yttrium Aluminum Garnet) fluorescent powder to prepare LED products with different optical parameters.

Description

Preparation and the application of the effective orange fluorescent powder of a kind of light-emitting diodes
Technical field
The present invention relates to preparation method and the Application Areas of the effective orange fluorescent powder of a kind of light-emitting diode.This fluorescent material can directly be excited by ultraviolet and blue chip, and sending peak wavelength is 570nm-580nm, and predominant wavelength is the orange-yellow spectrum of 580nm-590nm, can be applicable to indoor LED warm colour illumination.
Background technology
Tradition LED fluorescent material cooperates blue light or the compound white light that sends of ultraviolet chip, because fluorescent material mostly is yellow-green colour YAG fluorescent material, although it is wide to have a higher half-wave, owing to the disappearance of red spectrum, cause colour rendering index excessively low, can not directly apply to indoor LED warm colour illumination.In order to overcome this drawback, existing indoor warm light LED fluorescent material, mostly be to adopt with green and red LED fluorescent material to be used in conjunction with, significantly improved the color developing of product, but but caused the low problem of finished product luminous efficiency to produce, colleague's luminous efficiency has lowly also caused more energy to change into heat energy, has aggravated the LED components and parts and has reduced because of the life-span that heating causes.
If can be on the basis of existing YAG fluorescent material, develop and a kind ofly can effectively cover emitting red light interval, LED fluorescent material that luminous efficiency is high, will certainly cause a revolution of indoor warm optical illumination.
Be in above reason, improve by the prescription at traditional YAG yellow-green fluorescence powder, prepared a kind of LED YAG system orange fluorescent powder.
Its major advantage is: have preferably predominant wavelength and peak wavelength, and owing to being the improvement of carrying out on the basis of YAG fluorescent material, has luminous efficiency high, the wide advantage with stable performance of higher half-wave, can directly be combined with ultraviolet or blue chip and send white light, also can send white light on the well-mixed basis of YAG fluorescent material, being combined with ultraviolet and blue chip.
Summary of the invention
The present invention relates to preparation and the application of the effective orange fluorescent powder of a kind of light-emitting diode, the fluorescent material that a process for preparing is to improve on the basis of traditional YAG fluorescent material prescription, the effective orange fluorescent powder of a kind of light-emitting diodes that adopts high temperature solid-state method to prepare, it can send warm white in cooperating with ultraviolet and blue chip by effective application, or mix rear the cooperation with ultraviolet and blue chip with traditional YAG yellow-green fluorescence powder and send white light, its optical parametric can be regulated by the content that the present invention relates to fluorescent material.
The present invention realizes by the following technical solutions.
The preparation method of the effective orange fluorescent powder of a kind of light-emitting diode comprises the following aspects
1. the chemical formula of this fluorescent material is: (Y3-x-y, R x) Al 5O 12-k/2F k: Cey, wherein R is one or more among Ba, Gd, the Tb, F -Ion is introduced by fluorochemical, and wherein positively charged ion is one or both among Ba, the Al; 0.05≤X≤0.2,0.15≤y≤0.4,0.3≤K≤1.2 wherein is characterized in that this preparation method comprises following several step:
Selecting oxide compound or oxyhydroxide in the above-mentioned chemical formula is raw material, carries out quality according to the chemical formula component and takes by weighing, and each component after taking by weighing is tentatively mixed, and puts into planetary ball mill and carries out ball milling, and it is 24 hours that Ball-milling Time is set; Put into loft drier after the powder taking-up that will mix, set temperature is 110 ℃ dries, and drying time is the 8 little front work in-process of sintering of namely preparing; Work in-process before the sintering are placed in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1400 ℃-1600 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process; Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
2. described according to claim 1: wherein R is one or more among Ba, Gd, the Tb.
3. described according to claim 1: F wherein -Ion is introduced by fluorochemical, and wherein positively charged ion is Ba 2+, Al 3+In one or both.
4. described according to claim 1: 0.05≤X≤0.2,0.15≤y≤0.4,0.3≤K≤1.2.
5. described according to claim 1: as need to carry out 24 hours ball-milling processing to raw material.
6. described according to claim 1: sintering temperature is between 1400 ℃-1600 ℃.
7. the fluorescent material of the present invention's preparation can directly be excited by ultraviolet and blue light, and sending peak wavelength is 570nm-580nm, and predominant wavelength is the orange-yellow spectrum of 580nm-590nm.
8. the fluorescent material of the present invention's preparation encapsulates with ultraviolet and blue chip, can prepare the required illuminating product of warm white LED illumination system.
9. the fluorescent material of the present invention preparation can encapsulate with ultraviolet and blue chip with after conventional yellow YAG fluorescent material mixes, and can effectively improve the optical parametrics such as colour temperature, chromaticity coordinates of conventional fluorescent powder, prepares the White-light LED illumination product of different demands.
Description of drawings:
Fig. 1 is the exciting light spectrogram of example 2.
Fig. 2 is the utilizing emitted light spectrogram of example 2.
Fig. 3 is commercially available YAG fluorescent material and example 2 emmission spectrum comparison diagrams.
Fig. 4 is the emmission spectrum comparison diagram of example 5,6,7,9 different ingredients.
Fig. 5 be example 3,4,8, the utilizing emitted light spectrogram.
Embodiment:
Example 1
Take by weighing purity and be 99.99% and above raw material: Y 2O 359.83g, AL 2O 350.87g, CeO 25.1636g, Gd 2O 37.2499g, AlF 33H 2O 1.3797g puts into ball grinder, adopts planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 2
Take by weighing purity and be 99.99% and above raw material: Y 2O 357.36g, AL 2O 350.87g, CeO 210.3272g, Gd 2O 35.4374g, AlF 33H 2O 1.3797g, BaF 21.7533g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 3
Take by weighing purity and be 99.99% and above raw material: Y 2O 357.20g, AL 2O 349.75g, CeO 27.2289g, Gd 2O 36.887g, AlF 33H 2O 3.31g, BaF 23.506g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 4
Take by weighing purity and be 99.99% and above raw material: Y 2O 357.20g, AL 2O 349.75g, CeO 27.2289g, Gd 2O 36.887g, AlF 33H 2O 5.151g puts into ball grinder, adopts planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 5
Take by weighing purity and be 99.99% and above raw material: Y 2O 355.69g, AL 2O 349.75g, CeO 210.3271g, Gd 2O 33.62g, AlF 33H 2O 5.151g, BaF 23.506g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 6
Take by weighing purity and be 99.99% and above raw material: Y 2O 357.35g, AL 2O 349.75g, CeO 27.228g, Gd 2O 35.4374g, AlF 33H 2O 2.7594g, BaF 22.6299g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 7
Take by weighing purity and be 99.99% and above raw material: Y 2O 355.32g, AL 2O 348.94g, CeO 213.7695g, Gd 2O 31.8124g, AlF 33H 2O 2.7594g, BaF 21.7532g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 8
Take by weighing purity and be 99.99% and above raw material: Y 2O 356.90g, AL 2O 348.94g, CeO 27.228g, Gd 2O 36.1624g, AlF 33H 2O 1.3797g, BaF 22.6299g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
Example 9
Take by weighing purity and be 99.99% and above raw material: Y 2O 360.96g, AL 2O 347.96g, CeO 23.4423g, Gd 2O 39.0624g, AlF 33H 2O 2.5976g, BaF 23.6279g, put into ball grinder, adopt planetary ball mill to carry out ball milling 24 hours.The powder that mixes is put into loft drier, and set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours.Work in-process before the sintering are inserted in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1460 ℃, and soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process.Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.

Claims (9)

1. the present invention relates to preparation and the application of the effective orange fluorescent powder of a kind of light-emitting diode; The chemical formula of this fluorescent material is: (Y3-x-y, R x) Al 5O 12-k/2F k: Cey, wherein R is one or more among Ba, Gd, the Tb, F -Ion is introduced by fluorochemical, and wherein positively charged ion is one or both among Ba, the Al; 0.05≤X≤0.2,0.15≤y≤0.4,0.3≤K≤1.2 wherein.
2. described according to claim 1: wherein R is one or more among Ba, Gd, the Tb.
3. described according to claim 1: F wherein -Ion is introduced by fluorochemical, and wherein positively charged ion is Ba 2+, Al 3+In one or both.
4. described according to claim 1: 0.05≤X≤0.2,0.15≤y≤0.4,0.3≤K≤1.2.
5. the present invention adopts and is prepared as follows the method preparation:
Selecting oxide compound or oxyhydroxide in the above-mentioned chemical formula is raw material, carries out quality according to the chemical formula component and weighs, and after each component after taking by weighing is tentatively mixed, puts into planetary ball mill and carries out ball milling, and Ball-milling Time is 24 hours; Put into loft drier after the powder taking-up that will mix, set temperature is 110 ℃ dries, and dries namely to prepare the front work in-process of sintering in 8 hours; Work in-process before the sintering are placed in the corundum crucible, adopt box atmosphere furnace to carry out sintering, set temperature is 1400 ℃-1600 ℃; Soaking time is 8 hours, naturally cools to room temperature after sintering is finished and makes work in-process; Work in-process are sieved processing, can obtain required LED orange fluorescent powder finished product.
6. described according to claim 5: as need to carry out 24 hours ball-milling processing to raw material.
7. described according to claim 5: sintering temperature is between 1400 ℃-1600 ℃.
8. the fluorescent material of the present invention's preparation can directly be excited by ultraviolet and blue light, and sending peak wavelength is 570nm-580nm, and predominant wavelength is the orange-yellow spectrum of 580nm-590nm.
9. Application Areas of the present invention:
The fluorescent material of the present invention's preparation can encapsulate with ultraviolet and blue chip, with the required illuminating product of preparation warm white LED illumination system; The fluorescent material of the present invention preparation can encapsulate with ultraviolet and blue chip with after conventional yellow YAG fluorescent material mixes, and can effectively improve the optical parametrics such as colour temperature, chromaticity coordinates of conventional fluorescent powder, prepares the White-light LED illumination product of different demands.
CN 201210574859 2012-07-05 2012-12-27 Preparation and application of orange-yellow fluorescent powder for light-emitting diode Pending CN102994090A (en)

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CN 201210574859 CN102994090A (en) 2012-07-05 2012-12-27 Preparation and application of orange-yellow fluorescent powder for light-emitting diode

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104130779A (en) * 2014-07-01 2014-11-05 南京大学 Yellow fluorescent powder used for white light LED and preparation method thereof
CN105062481A (en) * 2015-07-15 2015-11-18 昆山开威电子有限公司 Red light-fluorescent light conversion material for plant lamp and preparation method of conversion material
CN111675492A (en) * 2020-05-21 2020-09-18 中国计量大学 High-color-rendering-property mixed fluorescent glass film for laser, preparation method thereof and thickness pre-screening method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104130779A (en) * 2014-07-01 2014-11-05 南京大学 Yellow fluorescent powder used for white light LED and preparation method thereof
CN105062481A (en) * 2015-07-15 2015-11-18 昆山开威电子有限公司 Red light-fluorescent light conversion material for plant lamp and preparation method of conversion material
CN111675492A (en) * 2020-05-21 2020-09-18 中国计量大学 High-color-rendering-property mixed fluorescent glass film for laser, preparation method thereof and thickness pre-screening method
CN111675492B (en) * 2020-05-21 2022-05-27 中国计量大学 High-color-rendering-performance mixed fluorescent glass film for laser, preparation method thereof and thickness pre-screening method

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Application publication date: 20130327