CN106565216A - Fireproof and fluorescent ceramic base for high-power LED, and preparation method thereof - Google Patents
Fireproof and fluorescent ceramic base for high-power LED, and preparation method thereof Download PDFInfo
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- CN106565216A CN106565216A CN201610929720.5A CN201610929720A CN106565216A CN 106565216 A CN106565216 A CN 106565216A CN 201610929720 A CN201610929720 A CN 201610929720A CN 106565216 A CN106565216 A CN 106565216A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052582 BN Inorganic materials 0.000 claims abstract description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 8
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 8
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 8
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 4
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000011863 silicon-based powder Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 235000015895 biscuits Nutrition 0.000 claims description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000002242 deionisation method Methods 0.000 claims 1
- 238000005299 abrasion Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 239000011222 crystalline ceramic Substances 0.000 description 6
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 6
- 241001025261 Neoraja caerulea Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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Abstract
The invention discloses a fireproof and fluorescent ceramic base for high-power LED, and a preparation method thereof, wherein the fireproof and fluorescent ceramic base is prepared from the following raw materials by weight: 2-3 parts of boron nitride, 1-2 parts of CeO2, 1-2 parts of cordierite, 40-50 parts of Al2O3, 4-7 parts of Y2O3, 3-6 parts of citric acid, 3-5 parts of ethylenediamine, 15-20 parts of deionized water, 1-2 parts of lanthanum oxide, 2-3 parts of tetraethyl orthosilicate, 1-2 parts of MgO, 30-40 parts of ethanol, 5-10 parts of silicon micro-powder, and 15-20 parts of a silane coupling agent KH550. According to the present invention, the fireproof and fluorescent ceramic base has functions of excellent tensile strength, excellent compressive strength, excellent abrasion resistance, high thermal conductivity, and fluorescence, wherein the fire resistance of the material is improved by matching with the added boron nitride and the like.
Description
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 fire resisting, can fluorescence pottery
Porcelain 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 scattering and absorption of the fluorescent material to light, 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 transmissivity, 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,
Thermal 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
Photostability and service life.
Shi Yun exists《Ce:Y3Al5O12Application study 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 thermal conductivity factor 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 thermal conductivity factor 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 fire resisting, can fluorescence base of ceramic, it is characterised in that be made up of the raw material of following weight portion：
Boron nitride 2-3, CeO2 1-2, cordierite 1-2, Al2O3 40-50, Y2O3 4-7, citric acid 3-6, ethylenediamine 3-5, go from
Sub- water 15-20, lanthana 1-2, 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 fire resisting, can fluorescence base of ceramic and preparation method thereof, it is characterised in that be by with
Lower step is made：
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, lanthana, boron nitride 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 box 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 fire resisting, can fluorescence base of ceramic and preparation method thereof, it is characterised in that step
Suddenly the vacuum of the vacuum drying oven described in d is（5-15）10-4Par。
The invention has the beneficial effects as follows：Silicon powder adsorptivity, the dispersiveness that Silane coupling agent KH550 was processed preferably, is soaked
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, compression strength, and anti-wear performance is improved, and can be increased
Big its thermal conductivity factor, increases fire resistance；Coordinate boron nitride of addition etc., improve the fire-resistance property of material.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.
Embodiment
A kind of great power LED fire resisting, can fluorescence base of ceramic, it is characterised in that be by the raw material of following weight portion
Make：
Boron nitride 3, CeO2 2, cordierite 2, Al2O3 50, Y2O3 7, citric acid 6, ethylenediamine 5, deionized water 20, lanthana 2,
Tetraethyl orthosilicate 3, MgO 2, ethanol 40, silicon powder 10, Silane coupling agent KH550 20；
A kind of described great power LED fire resisting, can fluorescence base of ceramic and preparation method thereof, it is characterised in that be by with
Lower step is made：
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, lanthana, boron nitride 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 box 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 fire resisting, can fluorescence base of ceramic and preparation method thereof, it is characterised in that step
Suddenly the vacuum of the vacuum drying oven described in 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 fire resisting, can fluorescence base of ceramic, it is characterised in that be by the raw material system of following weight portion
Into：
Boron nitride 2-3, CeO2 1-2, cordierite 1-2, Al2O3 40-50, Y2O3 4-7, citric acid 3-6, ethylenediamine 3-5, deionization
Water 15-20, lanthana 1-2, 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 fire resisting according to claim 1, can fluorescence base of ceramic and preparation method thereof, its
It is characterised by, 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, lanthana, boron nitride 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 box 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 fire resisting according to claim 2, can fluorescence base of ceramic and preparation method thereof, its
It is characterised by, the vacuum of the vacuum drying oven described in step d is（5-15）10-4Par。
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Application publication date: 20170419 |