CN104844217A - Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source - Google Patents
Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source Download PDFInfo
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- 229910017109 AlON Inorganic materials 0.000 title claims abstract description 60
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000004806 packaging method and process Methods 0.000 title abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 32
- 235000015895 biscuits Nutrition 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 238000005238 degreasing Methods 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910002106 crystalline ceramic Inorganic materials 0.000 claims description 23
- 239000011222 crystalline ceramic Substances 0.000 claims description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- -1 polyoxyethylene Polymers 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 235000006491 Acacia senegal Nutrition 0.000 claims description 4
- 241000978776 Senegalia senegal Species 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 4
- 239000000499 gel Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 235000021323 fish oil Nutrition 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 239000001856 Ethyl cellulose Substances 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 2
- 150000001241 acetals Chemical class 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 2
- 229920001249 ethyl cellulose Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 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 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920000193 polymethacrylate Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 239000011261 inert gas Substances 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 238000000498 ball milling Methods 0.000 abstract description 4
- 229910052593 corundum Inorganic materials 0.000 abstract description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 2
- 238000000137 annealing Methods 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 238000005538 encapsulation Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000004643 material aging Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention relates to a preparation method of an AlON transparent ceramic phosphor for a warm color temperature white light LED packaging light source. The method comprises the following steps: with Al powder and Al2O3The powder is taken as a raw material, added with absolute ethyl alcohol, ball-milled and uniformly mixed, dried, ground, sieved or spray-dried; placing the raw materials obtained by granulation in a crucible and sintering in a carbon furnace by nitrogen; crushing the sintered powder, adding rare earth oxide, sintering aid, binder, dispersant and liquid medium, and ball milling; obtaining a biscuit by adopting different molding modes according to the requirements of LED packaging on the shape specification or structure of the phosphor; degreasing the formed biscuit, and then placing the degreased biscuit in a carbon furnace for nitrogen sintering; and annealing and polishing the sintered ceramic to obtain the AlON transparent ceramic phosphor. The AlON transparent ceramic phosphor provided by the invention is used for LED packaging, the packaging structure is obviously simplified, the cost is reduced, and the overall optimization of the color temperature, the display finger and the lighting effect of an LED packaging light source is realized.
Description
Technical field
The present invention relates to a kind of preparation method of the AlON crystalline ceramics fluor for warm colour temperature white-light LED encapsulation light source, belong to transparent fluorescent ceramic preparing technical field.
Background technology
Photodiode (LED) semiconductor lighting has the plurality of advantages such as light efficiency is high, life-span length, environmental protection, save energy, is described as the revolutionary technology in new solid light source epoch 21 century.
Traditional white-light LED encapsulation material is fluorescent material, can show the defect that colour rendering index is too low, and fluorescent material and the aging look caused of packaging plastic drifts about and a difficult problem for light decay.
AlON base transparent ceramic has excellent optical property, chemical property, mechanical property and dielectric properties, and high thermal resistance is good, heat-resistant knocking stability is high and erosion-resisting characteristics is strong.Rear-earth-doped AlON crystalline ceramics fluor has that emission wavelength is adjustable, free of surface defects, high-quantum efficiency, without the advantage such as aging, low light attenuation, high permeability, and this system fluor can launch the ruddiness of 580nm-600nm, make up the blank of current fluorescent ceramic material, it is a kind of desirable fluorescent material, light source reliability and light efficiency can be significantly improved, without the need to fluorescent material and packaging plastic, significantly simplify encapsulating structure, reduce cost, having broken traditional LED route, is very potential white-light LED encapsulation material.
At present about the report of AlON base ceramic phosphor is little.(the Fang Zhang such as Zhang Fang, Xianyuan Yuan, Shaohua Wang, Shiwei Wang*.Preparation and luminescence properties of Eu2+doped γ-aluminum oxynitride transparent ceramics.Journal of Luminescence, 133 (2013) 200-202) with Al2O3 powder, AlN powder and Eu2O3 powder for raw material, adopt solid-phase synthesis to prepare the AlON:Eu2+ crystalline ceramics fluor of different levels of doping.This line fluorescent body has two emission peaks, one at 401nm, another emission peak is along with the increase generation red shift of Eu ion doping concentration.
This author (Fang Zhang, Liqiong An, Xuejian Liu, Guohong Zhou, Xianyang Yuan, Shiwei Wang.Upconversion Luminescence in γ-AlON:Yb
3+, Tm
3+ceramic Phosphors.J.Am.Ceram.Soc., 92 [8] 1888 – 1890 (2009)) be investigated Yb
3+, Tm
3+converting ceramic material on the AlON base of codoped, has the blue light of 479 and the red emission peak of 650nm under 980nm shooting conditions.
In addition this author (Zhang, F, Wang, SW, Liu, XJ, An, LQ, Yuan, XY.UpconversionLuminescence in Er-doped gamma-AlON ceramic phosphors.JOURNAL OF APPLIEDPHYSICS, 105,093542 (2009)) have studied the AlON powder prepared with carbothermic method for raw material, doping Er
2o
3, converting ceramic material in 1850 DEG C of synthesis, has the green glow of 548 and the red emission peak of 666nm under 980nm shooting conditions.
Summary of the invention
The object of this invention is to provide a kind of preparation method of the AlON crystalline ceramics fluor for warm colour temperature white-light LED encapsulation light source, obtain applications well in ultra-high efficiency lighting LED encapsulation field.
On the one hand, the invention provides a kind of preparation method of the AlON crystalline ceramics fluor for warm white LED packaged light source, it comprises the steps:
By Al powder and Al
2o
3after powder is mixed by wet ball grinding, drying and grinding, excessively 100 ~ 300 mesh sieves, obtain mixing raw material;
By described raw materials for sintering in nitrogen atmosphere, sinter at 1600 ~ 1900 DEG C, obtain AlON ceramic powder;
After described AlON ceramic powder is pulverized, add rare earth oxide, sintering aid, binding agent and dispersion agent, after carrying out wet ball grinding, obtain slurry;
To the specification requirement of AlON ceramic phosphor, described slurry is carried out shaping according to LED, obtain AlON biscuit of ceramics;
After described AlON biscuit of ceramics is carried out degreasing, under vacuum, carry out buried powder by the boron nitride crossed through 1800 ~ 2000 DEG C of pyroprocessing, be then placed in nitrogen atmosphere, sinter at 1800 ~ 2000 DEG C, obtain AlON crystalline ceramics;
After described AlON crystalline ceramics is carried out polished finish, obtain AlON crystalline ceramics fluor.
Preferably, the purity of described Al powder is 99.9%, described Al
2o
3the purity of powder is 99.99%.
Preferably, the forming method of described AlON biscuit of ceramics is dry-pressing formed, flow casting molding, injection forming, injection moulding or gel forming.As can be adopted dry-pressing formed, flow casting molding or injection forming for slice-shaped, bar shaped; Gel forming, injection moulding or injection forming can be adopted for semisphere.
Preferably, described rare earth oxide is selected from Ce
2o
3, Eu
2o
3, Er
2o
3, Pr
2o
3, Tb
2o
3in at least one.
Described sintering aid to be sintering aid be in yttrium oxide, magnesium oxide, lanthanum trioxide one or several.
Preferably, described binding agent is one or several in polyoxyethylene glycol, Sudan Gum-arabic, polyvinyl butyral acetal, polyvinyl alcohol, ethyl cellulose, ammonium polymethacrylate etc.
Preferably, described dispersion agent is one or several in oleic acid, fish oil, Viscotrol C, gelatin, Sudan Gum-arabic, polyoxyethylene glycol, polyethylene, polyoxyethylene glycol, polyacrylic acid etc.
Preferably; the degreasing method of described AlON biscuit of ceramics is be that shaping biscuit is put into crucible; again crucible and biscuit are loaded in tube furnace or box-type furnace; pass into oxygen and carry out atmosphere protection; 0.1 ~ 15 DEG C/min is adopted to be warmed up to 600 ~ 800 DEG C; and be incubated 5 ~ 50h, according to size and the organic materialization decision soaking time of biscuit.
Preferably, it is the thickness carrying out with 80 ~ 2000 order carborundum discs the pottery sintered be thinned to needs that described AlON crystalline ceramics carries out polished finish, then carries out mirror polish process with rubbing paste to thinning ceramic surface.
Second aspect, present invention also offers a kind of AlON composite transparent ceramic fluor for warm white LED packaged light source, and it is formed by stacking by multilayered fluorescent biscuit of ceramics or fluorescence ceramics biscuit and non-fluorescence biscuit of ceramics.
Compared with prior art, the present invention has following beneficial effect:
The AlON crystalline ceramics fluor of 580 ~ 600nm ruddiness that sets out can be prepared according to method of the present invention, can be used for low colour temperature height aobvious finger white-light LED encapsulation.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the AlON crystalline ceramics transmittance curve of embodiment 1 gained;
Fig. 2 is the AlON crystalline ceramics photo in kind of embodiment 1 gained.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
(1) by purity be 99.9% Al powder and purity be the Al of 99.99%
2o
3for raw material, both mass percents are 8:92.With Al powder and Al
2o
3the powder total amount of powder composition is benchmark, and add 1.1 times of dehydrated alcohols, with high purity aluminium oxide ball for abrading-ball, ball quality is 2 times of powder total amount, puts into polytetrafluoro tank ball milling 20h together.The slurry that ball milling is good dries 24h in 60 DEG C of baking ovens, more ground 200 orders;
(2) mixing raw material step (1) obtained is placed in boron nitride crucible and is sintered at carbon stove, after being evacuated to 10-2Pa, close vacuum pump and be filled with high pure nitrogen, nitrogen compressing tablet in stove is made to keep 1 ~ 2 normal atmosphere, with 5 DEG C/min be warming up to 1800 DEG C insulation 5h after furnace cooling, obtain AlON ceramic powder;
(3) after the AlON ceramic powder that step (2) obtains being carried out comminution by gas stream, with the AlON ceramic powder total amount obtained for benchmark, sintering aid 0.1wt%Y is added
2o
3+ 0.1wt%MgO+0.05wt%La
2o
3, add binding agent 0.8wt%PVB, add dispersion agent 0.3wt% fish oil, and add 110wt% dehydrated alcohol, polytetrafluoro tank ball milling 20h put into by 200wt% high purity aluminium oxide ball;
(4) ceramic size that step (3) obtains is carried out mist projection granulating, the ceramic powder particle diameter of acquisition is about 30um, then on tabletting machine, obtains disc AlON biscuit so that the pressure of 50MPa is dry-pressing formed;
(5) the AlON biscuit that step (4) obtains is put into carbon stove after 700 DEG C of skimming treatments, and by the boron nitride powder buried powder through pyroprocessing, be evacuated to 10
-2after Pa, close vacuum pump and be also filled with high pure nitrogen, make nitrogen pressure in furnace keep 1 ~ 2 normal atmosphere, be warming up to furnace cooling after 1930 DEG C of insulation 10h with 5 DEG C/min, obtain AlON crystalline ceramics.
(6), after the AlON pottery that step (5) obtains being carried out twin polishing process, obtain AlON crystalline ceramics, see Fig. 1; The transmitance of AlON pottery reaches 83.39%, sees Fig. 2.
embodiment 2
Other steps are identical with embodiment 1, unlike step (3) and step (4).0.15at%Ce is added again in the basis of embodiment 1 step (3)
2o
3, other are identical.Afterwards the ceramic size that step (3) obtains is carried out gel forming and obtain hemispheric AlON biscuit.Then carry out skimming treatment to sinter again.Sintering temperature is 1880 DEG C of insulation 10h.The semisphere Ce:AlON crystalline ceramics fluor obtained.
embodiment 3
Other steps are identical with embodiment 2, unlike step (4).The ceramic size that step (3) obtains is carried out the AlON biscuit that flow casting molding obtains bar shaped.Then carry out skimming treatment to sinter again.Sintering temperature is 1880 DEG C of insulation 10h.The bar shaped Ce:AlON crystalline ceramics fluor obtained.
embodiment 4
Other steps are identical with embodiment 1, unlike step (5).Put into carbon stove after disc AlON biscuit 700 DEG C of skimming treatments step (4) obtained, and by the boron nitride powder buried powder through pyroprocessing, be evacuated to 10
-2after Pa, close vacuum pump and be also filled with high pure nitrogen, make nitrogen pressure in furnace keep 1 ~ 2 normal atmosphere, be warming up to furnace cooling after 1930 DEG C of insulation 10h with 10 DEG C/min, obtain AlON pottery.By pottery after twin polishing process, obtain the AlON crystalline ceramics that transmitance is 80%.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (9)
1., for a preparation method for the AlON crystalline ceramics fluor of warm white LED packaged light source, it is characterized in that, comprise the steps:
By Al powder and Al
2o
3after powder is mixed by wet ball grinding, drying and grinding, excessively 100 ~ 300 mesh sieves, obtain mixing raw material;
By described raw materials for sintering in nitrogen atmosphere, sinter at 1600 ~ 1900 DEG C, obtain AlON ceramic powder;
After described AlON ceramic powder is pulverized, add rare earth oxide, sintering aid, binding agent and dispersion agent, after carrying out wet ball grinding, obtain slurry;
To the specification requirement of AlON ceramic phosphor, described slurry is carried out shaping according to LED, obtain AlON biscuit of ceramics;
After described AlON biscuit of ceramics is carried out degreasing, under vacuum, carry out buried powder by the boron nitride crossed through 1800 ~ 2000 DEG C of pyroprocessing, be then placed in nitrogen atmosphere, sinter at 1800 ~ 2000 DEG C, obtain AlON crystalline ceramics;
After described AlON crystalline ceramics is carried out polished finish, obtain AlON crystalline ceramics fluor.
2. preparation method according to claim 1, is characterized in that, the forming method of described AlON biscuit of ceramics is dry-pressing formed, flow casting molding, injection forming, injection moulding or gel forming.
3. preparation method according to claim 1, is characterized in that, described rare earth oxide is selected from Ce
2o
3, Eu
2o
3, Er
2o
3, Pr
2o
3, Tb
2o
3in at least one.
4. preparation method according to claim 1, is characterized in that, described sintering aid is one or several in yttrium oxide, magnesium oxide, lanthanum trioxide.
5. preparation method according to claim 1, is characterized in that, described binding agent is one or several in polyoxyethylene glycol, Sudan Gum-arabic, polyvinyl butyral acetal, polyvinyl alcohol, ethyl cellulose, ammonium polymethacrylate etc.
6. preparation method according to claim 1, is characterized in that, described dispersion agent is one or several in oleic acid, fish oil, Viscotrol C, gelatin, Sudan Gum-arabic, polyoxyethylene glycol, polyethylene, polyoxyethylene glycol, polyacrylic acid etc.
7. preparation method according to claim 1; it is characterized in that; the degreasing of described AlON biscuit of ceramics is that shaping biscuit is put into crucible; again crucible and biscuit are loaded in tube furnace or box-type furnace; 0.1 ~ 15 DEG C/min is adopted to be warmed up to the organic decomposition temperature of interpolation; and be incubated 5 ~ 50h, according to size and the organic materialization decision soaking time of biscuit, oxygen atmosphere can be utilized to protect or protection of inert gas degreasing.
8. preparation method according to claim 1, it is characterized in that, it is the thickness carrying out with 80 ~ 2000 order carborundum discs the pottery sintered be thinned to needs that described AlON crystalline ceramics carries out polished finish, then carries out mirror polish process with rubbing paste to thinning ceramic surface.
9. for an AlON composite transparent ceramic fluor for warm white LED packaged light source, it is characterized in that, the multilayered fluorescent biscuit of ceramics prepared by the method by claim 1 or fluorescence ceramics biscuit and non-fluorescence biscuit of ceramics are formed by stacking.
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|---|---|---|---|
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|---|---|---|---|
| CN201510152565.6A CN104844217B (en) | 2015-04-01 | 2015-04-01 | Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source |
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Cited By (12)
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| CN106145955A (en) * | 2016-08-08 | 2016-11-23 | 屠秀芬 | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN106242583A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of SiALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN106242577A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN106316381A (en) * | 2016-08-08 | 2017-01-11 | 屠秀芬 | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic |
| CN106478108A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of method preparing large scale AlON crystalline ceramics |
| WO2017157157A1 (en) * | 2016-03-18 | 2017-09-21 | 深圳市绎立锐光科技开发有限公司 | Method for preparing fluorescent ceramic provided with aluminum nitride substrate, and related fluorescent ceramic |
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| CN110272282A (en) * | 2019-06-28 | 2019-09-24 | 上海大学 | The low temperature preparation method of AlON crystalline ceramics |
| CN110386822A (en) * | 2018-04-19 | 2019-10-29 | 深圳光峰科技股份有限公司 | A kind of complex phase fluorescence ceramics and preparation method thereof |
| CN113979739A (en) * | 2021-10-27 | 2022-01-28 | 中国科学院上海硅酸盐研究所 | Composite fluorescent ceramic, preparation method and luminescent device |
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| CN106478108A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of method preparing large scale AlON crystalline ceramics |
| WO2017157157A1 (en) * | 2016-03-18 | 2017-09-21 | 深圳市绎立锐光科技开发有限公司 | Method for preparing fluorescent ceramic provided with aluminum nitride substrate, and related fluorescent ceramic |
| WO2017177923A1 (en) * | 2016-04-12 | 2017-10-19 | 深圳市绎立锐光科技开发有限公司 | Method for preparing fluorescent ceramic having aluminum oxide substrate, and related fluorescent ceramic |
| CN106316381A (en) * | 2016-08-08 | 2017-01-11 | 屠秀芬 | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic |
| CN106145955A (en) * | 2016-08-08 | 2016-11-23 | 屠秀芬 | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN106242577A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN106242583A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of SiALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN110386822A (en) * | 2018-04-19 | 2019-10-29 | 深圳光峰科技股份有限公司 | A kind of complex phase fluorescence ceramics and preparation method thereof |
| CN110386822B (en) * | 2018-04-19 | 2021-02-26 | 深圳光峰科技股份有限公司 | Complex phase fluorescent ceramic and preparation method thereof |
| CN109732841A (en) * | 2018-12-14 | 2019-05-10 | 安徽环嘉天一再生资源有限公司 | A kind of preparation method of uvioresistant plastic plate |
| CN109516813A (en) * | 2019-01-08 | 2019-03-26 | 大连海事大学 | A kind of method that direct water injection forming prepares high light transmittance AlON crystalline ceramics |
| CN109516813B (en) * | 2019-01-08 | 2021-04-23 | 大连海事大学 | Method for preparing high-light-transmittance AlON transparent ceramic by direct water injection molding |
| CN110272282A (en) * | 2019-06-28 | 2019-09-24 | 上海大学 | The low temperature preparation method of AlON crystalline ceramics |
| CN110272282B (en) * | 2019-06-28 | 2022-01-07 | 上海大学 | Low-temperature preparation method of AlON transparent ceramic |
| CN113979739A (en) * | 2021-10-27 | 2022-01-28 | 中国科学院上海硅酸盐研究所 | Composite fluorescent ceramic, preparation method and luminescent device |
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