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CN106565219A - Magnesium fluoride-doped and fluorescent ceramic base for high-power LED and preparation method for ceramic base - Google Patents

Magnesium fluoride-doped and fluorescent ceramic base for high-power LED and preparation method for ceramic base Download PDF

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Publication number
CN106565219A
CN106565219A CN201610971776.7A CN201610971776A CN106565219A CN 106565219 A CN106565219 A CN 106565219A CN 201610971776 A CN201610971776 A CN 201610971776A CN 106565219 A CN106565219 A CN 106565219A
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parts
ceramic base
afluon
asta
power led
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林琴
缪继平
周逢婷
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Anhui Zhong Wei Photoelectric Material Co Ltd
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Anhui Zhong Wei Photoelectric Material Co Ltd
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Abstract

The invention discloses a magnesium fluoride-doped and fluorescent ceramic base for a high-power LED and a preparation method for the ceramic base. The ceramic base is characterized by being prepared from the following raw materials in parts by weight: 2-3 parts of magnesium fluoride, 1-2 parts of CeO<2>, 30-40 parts of Al<2>O<3>, 4-7 parts of Y<2>O<3>, 1-2 parts of mullite, 3-6 parts of citric acid, 3-5 parts of ethylenediamine, 15-20 parts of deionized water, 1-3 parts of zirconium oxide, 2-3 parts of tetraethyl orthosilicate, 1-2 parts of MgO, 30-40 parts of ethyl alcohol, 5-10 parts of silica powder, and 15-20 parts of silane coupling agent KH550. The ceramic base disclosed by the invention has excellent tensile strength, compressive strength and abrasive resistance, high heat conduction coefficient, and the fluorescent function; and by virtue of the additional magnesium fluoride and the like, the overall scratching resistance can be improved under the premise of improving the anti-reflection effect of the material.

Description

A kind of great power LED doping Afluon (Asta), can fluorescence ceramics pedestal and its preparation Method
Technical field
The present invention relates to a kind of base of ceramic of LED, and in particular to a kind of great power LED doping Afluon (Asta), can Fluorescence ceramics pedestal and preparation method thereof.
Background technology
Crystalline ceramics as a kind of novel photoelectric functional material for developing rapidly in recent years, calorifics, mechanical property, Optical property, composite construction and large-scale production aspect is with the obvious advantage, and crystalline ceramics is at present mainly as window material, laser material Material and scintillation material are applied:The luminescent material of transparence can solve fluorescent material to scattering of light and absorption, improve luminous Efficiency;There is no the segregation coefficient of monocrystalline in ceramics, it is possible to achieve the high concentration of various light emitting ionics is uniformly co-doped with, so as to can By various parameters such as absorbance, the luminescence bands of precise control potsherd fluorophor, to adjust and control phosphor ceramic piece Ratio between the gold-tinted of conversion and the blue light do not changed, using the uniformity of crystalline ceramics itself, obtains homogeneous high-quality White light, and luminescent designs can be carried out, develop new material;Crystalline ceramics has an excellent mechanically and thermally mechanical property, anti-vibration, Heat conductivity is good, it is possible to resolve blue-ray LED persistently lights lower temperature and raises the various luminous problem for causing, and further improves sending out for device Light stability and service life.
Shi Yun exists《Ce:Y3Al5O12Applied research of the crystalline ceramics in white light LEDs》In, using CeO2、Al2O3 、Y2O3 A kind of crystalline ceramics is prepared for, but also be there are problems that heat conductivity is not good enough, do not had.
The content of the invention
Think deeply based on more than, the present invention is intended to provide a kind of heat conductivity is big, and the great power LED with fluorescent functional With base of ceramic and preparation method thereof.
The technical problem to be solved is realized using following technical scheme:
A kind of great power LED doping Afluon (Asta), can fluorescence ceramics pedestal, it is characterised in that be by the original of following weight portion Material is made:
Afluon (Asta) 2-3, CeO2 1-2, Al2O3 30-40, Y2O3 4-7, mullite 1-2, citric acid 3-6, ethylenediamine 3-5, go from Sub- water 15-20, zirconium oxide 1-3, tetraethyl orthosilicate 2-3, MgO1-2, ethanol 30-40, silicon powder 5-10, Silane coupling agent KH550 15-20;
A kind of described great power LED doping Afluon (Asta), can fluorescence ceramics pedestal and preparation method thereof, it is characterised in that It is made up of following steps:
A. with citric acid as carbon source, ethylenediamine, deionized water are added, is placed 3-7 days under the conditions of 150-250 DEG C, obtained in purple Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission;
B. silicon powder, mullite are added in step b gained liquid, add Silane coupling agent KH550, ultrasonic disperse 10- After 30min, 3-5h is soaked, filter, wash, dry, obtain adsorbing the mixture of carbon point fluorescent material;
C. by CeO2, Al2O3, Y2O3, Afluon (Asta), zirconium oxide and step a gained mixture add in ball mill, and add positive silicon Acetoacetic ester, MgO, ethanol, Jing after ball mill mixing 8-15h, slurry are placed in the drying baker that temperature is 80-120 DEG C and are fully done It is dry;
D. step c gains is sieved and make biscuit with isostatic cool pressing, then proceed to 1650 DEG C of -1850 DEG C of temperature in vacuum drying oven After lower insulation 20h, transparent sample can be obtained, be to eliminate the internal stress and Lacking oxygen that may be introduced during vacuum-sintering, will be tried Sample is annealed 15-25 h in 1380-1500 DEG C of air atmosphere.
A kind of described great power LED doping Afluon (Asta), can fluorescence ceramics pedestal and preparation method thereof, its feature exists In the vacuum of the vacuum drying oven described in step d is(5-15)10-4Par。
The invention has the beneficial effects as follows:Silicon powder adsorptivity, the dispersibility that Silane coupling agent KH550 was processed preferably, soaks After steeping in carbon point fluorescent material, carbon point fluorescent material can be adsorbed, so as to give encapsulating material can fluorescence the characteristics of, meanwhile, It is dispersed in ceramic bases, it is to avoid the directly contact of carbon point fluorescent material and LED chip, efficiently solve due to LED chips generate heat and cause the problem that fluorescent material rate of decay is too high, failure is too fast, and then improve the use of LED lamps Life-span and integrated quality;Meanwhile, silicon powder strengthens can the tension of ceramic base, comprcssive strength, and anti-wear performance is improved, and can be increased Big its heat conductivity, increases fire resistance;Coordinate Afluon (Asta) of addition etc., can carry on the premise of material antireflective effect is improved High whole its scratch resistant.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.
Embodiment
A kind of great power LED doping Afluon (Asta), can fluorescence ceramics pedestal, it is characterised in that be by following weight portion Raw material make:
Afluon (Asta) 3, CeO2 2, Al2O3 40, Y2O3 7, mullite 2, citric acid 6, ethylenediamine 5, deionized water 20, zirconium oxide 3, Tetraethyl orthosilicate 3, MgO2, ethanol 40, silicon powder 10, Silane coupling agent KH550 20;
A kind of described great power LED doping Afluon (Asta), can fluorescence ceramics pedestal and preparation method thereof, it is characterised in that It is made up of following steps:
A. with citric acid as carbon source, ethylenediamine, deionized water are added, is placed 3-7 days under the conditions of 150-250 DEG C, obtained in purple Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission;
B. silicon powder, mullite are added in step b gained liquid, add Silane coupling agent KH550, ultrasonic disperse 10- After 30min, 3-5h is soaked, filter, wash, dry, obtain adsorbing the mixture of carbon point fluorescent material;
C. by CeO2, Al2O3, Y2O3, Afluon (Asta), zirconium oxide and step a gained mixture add in ball mill, and add positive silicon Acetoacetic ester, MgO, ethanol, Jing after ball mill mixing 8-15h, slurry are placed in the drying baker that temperature is 80-120 DEG C and are fully done It is dry;
D. step c gains is sieved and make biscuit with isostatic cool pressing, then proceed to 1650 DEG C of -1850 DEG C of temperature in vacuum drying oven After lower insulation 20h, transparent sample can be obtained, be to eliminate the internal stress and Lacking oxygen that may be introduced during vacuum-sintering, will be tried Sample is annealed 15-25 h in 1380-1500 DEG C of air atmosphere.
A kind of described great power LED doping Afluon (Asta), can fluorescence ceramics pedestal and preparation method thereof, its feature exists In the vacuum of the vacuum drying oven described in step d is(5-15)10-4Par。
The present invention technical parameter be:Thermal conductivity >=15 W/mK;Light efficiency is more than or equal to 130 lm/W.

Claims (3)

1. a kind of great power LED doping Afluon (Asta), can fluorescence ceramics pedestal, it is characterised in that be by following weight portion Raw material is made:
Afluon (Asta) 2-3, CeO2 1-2, Al2O3 30-40, Y2O3 4-7, mullite 1-2, citric acid 3-6, ethylenediamine 3-5, deionization Water 15-20, zirconium oxide 1-3, tetraethyl orthosilicate 2-3, MgO1-2, ethanol 30-40, silicon powder 5-10, Silane coupling agent KH550 15-20。
2. a kind of great power LED doping Afluon (Asta) according to claim 1, can fluorescence ceramics pedestal and its preparation side Method, it is characterised in that be made up of following steps:
A. with citric acid as carbon source, ethylenediamine, deionized water are added, is placed 3-7 days under the conditions of 150-250 DEG C, obtained in purple Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission;
B. silicon powder, mullite are added in step b gained liquid, add Silane coupling agent KH550, ultrasonic disperse 10- After 30min, 3-5h is soaked, filter, wash, dry, obtain adsorbing the mixture of carbon point fluorescent material;
C. by CeO2, Al2O3, Y2O3, Afluon (Asta), zirconium oxide and step a gained mixture add in ball mill, and add positive silicon Acetoacetic ester, MgO, ethanol, Jing after ball mill mixing 8-15h, slurry are placed in the drying baker that temperature is 80-120 DEG C and are fully done It is dry;
D. step c gains is sieved and make biscuit with isostatic cool pressing, then proceed to 1650 DEG C of -1850 DEG C of temperature in vacuum drying oven After lower insulation 20h, transparent sample can be obtained, be to eliminate the internal stress and Lacking oxygen that may be introduced during vacuum-sintering, will be tried Sample is annealed 15-25 h in 1380-1500 DEG C of air atmosphere.
3. a kind of great power LED doping Afluon (Asta) according to claim 2, can fluorescence ceramics pedestal and its preparation side Method, it is characterised in that the vacuum of the vacuum drying oven described in step d is(5-15)10-4Par。
CN201610971776.7A 2016-11-07 2016-11-07 Magnesium fluoride-doped and fluorescent ceramic base for high-power LED and preparation method for ceramic base Pending CN106565219A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110981481A (en) * 2019-12-31 2020-04-10 江苏师范大学 Preparation method of stepped complex-phase fluorescent ceramics for high-efficiency white light LEDs
CN112210365A (en) * 2019-07-11 2021-01-12 天津大学 Method for preparing nano zirconium dioxide carbon quantum dot composite material by one-pot method

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CN103066186A (en) * 2013-01-07 2013-04-24 浙江华正新材料股份有限公司 Insulating layer and aluminum substrate of ceramic chip composite structure and manufacturing method of the same
CN103881438A (en) * 2014-02-14 2014-06-25 程实 Wear-resistant LED heat dispersion coating and preparation method thereof
CN105304793A (en) * 2015-10-08 2016-02-03 五邑大学 Insulated liquid packaged LED and preparation method thereof
CN105753483A (en) * 2014-12-17 2016-07-13 黄更生 Heat radiator ceramic material

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CN1573484A (en) * 2003-05-21 2005-02-02 株式会社半导体能源研究所 Liquid crystal display device
CN101697367A (en) * 2009-09-30 2010-04-21 烁光特晶科技有限公司 Method for preparing LED by using transparent ceramics
CN103066186A (en) * 2013-01-07 2013-04-24 浙江华正新材料股份有限公司 Insulating layer and aluminum substrate of ceramic chip composite structure and manufacturing method of the same
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Application publication date: 20170419