WO2008012712A1 - Yag-based ceramic garnet material comprising at least one multi-site element - Google Patents
Yag-based ceramic garnet material comprising at least one multi-site element Download PDFInfo
- Publication number
- WO2008012712A1 WO2008012712A1 PCT/IB2007/052725 IB2007052725W WO2008012712A1 WO 2008012712 A1 WO2008012712 A1 WO 2008012712A1 IB 2007052725 W IB2007052725 W IB 2007052725W WO 2008012712 A1 WO2008012712 A1 WO 2008012712A1
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- WIPO (PCT)
- Prior art keywords
- yag
- based ceramic
- garnet material
- systems
- ceramic garnet
- Prior art date
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- 239000000463 material Substances 0.000 title claims abstract description 99
- 239000000919 ceramic Substances 0.000 title claims abstract description 76
- 239000002223 garnet Substances 0.000 title claims abstract description 69
- 239000000203 mixture Substances 0.000 claims description 24
- 238000005245 sintering Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052727 yttrium Inorganic materials 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 6
- 229910010293 ceramic material Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 5
- 229910052691 Erbium Inorganic materials 0.000 claims description 5
- 229910052689 Holmium Inorganic materials 0.000 claims description 5
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052775 Thulium Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 44
- 230000000052 comparative effect Effects 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 239000000470 constituent Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 4
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000004814 ceramic processing Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000003826 uniaxial pressing Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
- C04B2235/81—Materials characterised by the absence of phases other than the main phase, i.e. single phase materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
Definitions
- the present invention is directed to ceramic garnet materials, especially those materials which are of use in the context of light emitting devices, especially of LEDs.
- LEDs comprise to a large extent Ce(III) doped YAG-based materials due to the excellent material properties of YAG.
- Ce(III) doped YAG-based materials due to the excellent material properties of YAG.
- it is e.g. referred to the US 2003 /0078156 Al which is hereby incorporated by reference.
- Y3AI5O12 crystallizes as a line compound with either alumina, AI2O3, or YAP, YAIO3, as neighboring phases that are formed in poly crystalline garnet YAG materials, if deviations from ideal stoichiometry occur.
- YAG Y3AI5O12
- Y3AI5O12 (YAG) garnet compound an excess of Y 2 O 3 or AI 2 O 3 , in Y3AI5O12 (YAG) garnet compound.
- Such anti-site disorder may lead to an extension of the single phase existence area surrounding the line compound stoichiometry especially for compositions showing an yttria excess because incorporation of yttrium at octahedral aluminum sites is energetically more favorable than incorporation of aluminium at dodecahedral yttrium sites.
- a YAG-based ceramic garnet material comprising at least one multi-site element capable of occupying the octahedral and/or the dodecahedral coordinated cation lattice sites inside the YAG-based ceramic garnet material.
- the production tolerance can be greatly enhanced without affecting the features of the YAG-based ceramic.
- the features of the YAG-based ceramic garnet material can even be improved.
- YAG-based especially means and/or includes a material which comprises as a main constituent a material M ⁇ M ⁇ M ⁇ X ⁇ with M 1 selected out of the group Mg, Ca, Y, Na, Sr, Gd, La, Ce, Pr, Nd, Sm, Eu, Dy, Tb, Ho, Er, Tm, Yb, Lu or mixtures thereof, M ⁇ selected out of the group Al, Ga, Mg, Zn, Y, Ge, Sc, Zr, Ti, Hf, Lu or mixtures thereof, M m selected out of the group Al, Si, B, Ge, Ga, V, As, Zn or mixtures thereof, X selected out of the group O, S, N, F, Cl, Br, I, OH and mixtures thereof and built of M 11 X 6 octahedra and M 111 X 4 tetrahedra in which each octahedron is joint to six others through vertex-sharing tetrahedra.
- each tetrahedron shares its vertices with four octahedra, so that the composition of the framework is (M 11 Xs) 2 (M 111 X 2 )S. Larger ions M 1 occupy positions of 8-coordination (dodecahedral) in the interstices of the framework, giving the final composition M ⁇ M ⁇ M ⁇ X ⁇ or M ⁇ M ⁇ M 11 ⁇ .
- main constituent means especially that > 95 %, preferably > 97 % and most preferred > 99 % of the YAG-based ceramic garnet material - without the at least one multisite element and possibly added dopant materials - consists out of this material. It should be noted that in some garnet materials within the present invention, the M ⁇ and M m positions are at least partly occupied by atoms of the same element.
- the YAG-based ceramic material may be doped with a material selected out of the group Lu, Pr, Sm, Tb, Dy, Ho, Er, Tm, Yb, La, Ce or mixtures thereof.
- YAG-based ceramic garnet material in the sense of the present invention furthermore means and/or includes especially a mixture of the material as described above with additives which may be added during ceramic processing. These additives may be incorporated fully or in part into the final material, which then may also be a composite of several chemically different species and particularly include such species known to the art as fluxes. Suitable fluxes include alkaline earth - or alkaline - metal oxides and halides, borates, SiO 2 and the like.
- ceramic material in the sense of the present invention means and/or includes especially a crystalline or polycrystalline compact material or composite material with a controlled amount of pores or which is pore free.
- polycrystalline material in the sense of the present invention means and/or includes especially a material with a volume density larger than 90 percent of the main constituent, consisting of more than 80 percent of single crystal domains, with each domain being larger than 0.5 ⁇ m in diameter and may have different crystallo graphic orientations.
- the single crystal domains may be connected by amorphous or glassy material or by additional crystalline constituents.
- the ionic radius for six fold coordination of the at least one multi-site element is > 70 pm to ⁇ 104 pm and/or the ionic radius for eight fold coordination of the at least one multi-site element is > 85 pm to ⁇ 116 pm. This has been shown in many applications within the present invention to be most efficient.
- the ionic radius for six- fold coordination of the at least one multi-site element is > 75 pm to ⁇ 104 pm, more preferred > 88 pm to ⁇ 102 pm.
- the ionic radius for eight-fold coordination of the at least one multi-site element is > 90 pm to ⁇ 114 pm, more preferred > 92 pm to ⁇ 112 pm.
- the concentration of the at least one multi-site element is > 0,5 mol% to ⁇ 5 mol% with respect to the YAG-based garnet structure. This has been shown to be the best suitable range in order to obtain the widest processing window without deteriorating the features of the YAG- material within a wide range of applications within the present invention.
- the concentration of the at least one multi-site element is > 0.1 atom% to ⁇ 0.7 atom%, preferably > 0.2 atom% to ⁇ 0.4 atom%, with respect to the sum of cations in the formula unit.
- the quotient of the sum of (Y, Lu, Gd, Pr, Sm, Tb, Dy, Ho, Er, Tm, Yb, La, Ce, Ca) and the sum of (Al, B, Si, Mg, Ge, Zr, Hf, Ga, Sc) in the ceramic garnet material is >0.590 to ⁇ 0.610.
- the ratio of the main phase towards possible secondary phase(s) in the YAG-based ceramic garnet material is >10 :1, preferably >20 :1 and most preferred >40 :1
- second phase in the sense of the present invention especially means and/or includes a minor constituent of the final mixture exhibiting different chemical composition and/or crystal structure.
- the at least one multi-site element is selected out of the group comprising Sc, Ga, Yb, Lu, Mg and mixtures thereof. These materials have proven themselves in practice in many applications.
- the photothermal stability of the Ce(III) doped YAG-based ceramic garnet material is >80% to ⁇ 100% after exposure of the ceramic material for 1000 hrs at 200 0 C with a light power density of 10W/cm 2 and an average photon energy of 2.75 eV.
- photothermal stability in the sense of the present invention especially means and/or includes the conservation of the luminescence intensity under simultaneous application of heat and high intensity excitation, i.e. a photothermal stability of 100% indicates that the material is virtually unaffected by the simultaneous irradiation and heat up.
- the photothermal stability of the Ce(III) doped YAG-based ceramic garnet material is
- the thermal conductivity of the YAG-based ceramic garnet material is > 0.07 W Cm 1 K "1 to ⁇ 0.15 W Cm 1 K "1
- the quantum yield of a Ce(III) doped YAG [PS i]-based ceramic garnet material is > 90% to ⁇ 99%
- the term "quantum yield" in the sense of the present invention especially means and/or includes the ratio of the number of photons emitted to the number of photons absorbed.
- the quantum yield of the YAG-based ceramic garnet material is > 93% to ⁇ 99%, preferably > 95% to ⁇ 98% According to one embodiment of the present invention, the YAG-based ceramic garnet material shows a transparency for normal incidence in air of >10 % to ⁇ 85 % for light in the wavelength range from > 550 nm to ⁇ 1000 nm.
- the transparency for normal incidence is in air of >20 % to ⁇ 80 % for light in the wavelength range from > 550 nm to ⁇ 1000 nm, more preferred >30 % to ⁇ 75 % and most preferred > 40% to ⁇ 70% for a light in the wavelength range from > 550 nm to ⁇ 1000 nm.
- transparency in the sense of the present invention means especially that > 10% preferably >20%, more preferred >30%, most preferred >40% and ⁇ 85% of the incident light of a wavelength, which cannot be absorbed by the material, is transmitted through the sample for normal incidence in air (at an arbitrary angle). This wavelength is preferably in the range of > 550 nm and ⁇ 1000 nm.
- the YAG- based ceramic garnet material has a density of >95% and ⁇ 101% of the theoretical density of the stoichiometric garnet structure. According to a preferred embodiment of the present invention, the YAG- based ceramic garnet material has a density of >97% and ⁇ 100% of the theoretical density.
- the densities lower than 100% according to the described preferred embodiment of the present invention are preferably obtained by sintering of the ceramic to a stage where still pores are present in the ceramic matrix. Most preferred are densities in the range >98.0% and ⁇ 99.8% with total pore volumes in the ceramic matrix within the >0.2 - ⁇ 2% range. A preferred mean pore diameter is in the >400 - ⁇ 1500 nm range.
- the present invention furthermore relates to a method of producing a
- YAG-based ceramic garnet material comprising a sintering step.
- the term "sintering step" in the sense of the present invention means especially densif ⁇ cation of a precursor powder under the influence of heat, which may be combined with the application of uniaxial or isostatic pressure, without reaching the liquid state of the main constituents of the sintered material.
- the sintering step is pressureless, preferably in reducing or inert atmosphere.
- the method furthermore comprises the step of pressing the ceramic garnet precursor material to >50% to ⁇ 70 %, preferably >55% to ⁇ 65 %, of its theoretical density before sintering. It has been shown in practice that this improves the sintering steps for most YAG-based ceramic garnet materials as described with the present invention.
- the method of producing a YAG-based ceramic garnet material according to the present invention comprises the following steps:
- a first pressing step preferably a unixial pressing step using a suitable powder compacting tool with a mould in the desired shape (e.g. rod- or pellet- shape) and/ or a cold isostatic pressing step preferably at >3000 bar to ⁇ 5000 bar.
- an optional hot pressing step preferably a hot isostatic pressing step preferably at >30 bar to ⁇ 2500 bar and preferably at a temperature of >1500 0 C to ⁇ 2000 0 C and/or a hot uniaxial pressing step preferably at >100 bar to ⁇ 2500 bar and preferably at a temperature of >1500 0 C to ⁇ 2000 0 C.
- a post annealing step at >1000°C to ⁇ 1700 0 C in inert atmosphere or in an oxygen containing atmosphere.
- this production method has produced the best YAG-based ceramic garnet materials as used in the present invention.
- the present invention also relates to a light emitting device, especially a LED comprising a YAG-based ceramic garnet material of the present invention.
- a YAG-based ceramic garnet material according to the present invention a light emitting device comprising a YAG-based ceramic garnet material according to the present invention and/or a YAG-based ceramic garnet material as produced with the present method may be of use in a broad variety of systems and/or applications, amongst them one or more of the following:
- Office lighting systems household application systems - shop lighting systems, home lighting systems, accent lighting systems, spot lighting systems, theatre lighting systems, - fiber-optics application systems, projection systems, self-lit display systems, pixelated display systems, segmented display systems, - warning sign systems, medical lighting application systems, indicator sign systems, and decorative lighting systems portable systems - automotive applications green house lighting systems window materials and window applications laser applications systems, especially for polycrystalline laser materials with garnet host lattice light emitting device housings, especially for HID lamps - optical lenses or elements with high refractive index
- Fig. 1 shows a microstructure of a YAG-based ceramic garnet material according to Example I of the present invention
- Fig. 2 shows a microstructure of a YAG-based ceramic garnet material according to Example II of the present invention
- Fig. 3 shows a microstructure of a YAG-based ceramic garnet material according to Example III of the present invention
- Fig.4 shows a microstructure of a YAG-based ceramic garnet material according to Example IV of the present invention
- Fig. 5 shows a microstructure of a YAG ceramic garnet material according to Comparative Example I
- Fig. 6 shows a microstructure of a YAG ceramic garnet material according to Comparative Example II
- Fig. 7 shows a microstructure of a YAG ceramic garnet material according to Comparative Example III
- Fig. 8 shows a microstructure of a YAG ceramic garnet material according to Comparative Example IV
- the garnet materials were made the following way: First, the appropriate amounts of powders of Y2O3 (99.99%, Rhodia),
- Gd 2 O 3 (99.99%, Rhodia), Sc 2 O 3 (99.9%) , Al 2 O 3 (99,99%, Baikowski) and CeO 2 (> 99%, Rhodia) were weighed in and milling with high density alumina milling media in isopropanol with 1000 ppm silica added as hydro lyzed tetraethoxysilane was carried out. Afterwards, the ceramic slurry was sieved to remove coarser particles and dried after addition of a polyvinylbutyral based binder system. The powder mixture was then granulated and ceramic green bodies were formed by means of cold isostatic pressing.
- Table I shows the material compositions of the four inventive Examples I to IV: Table 1 : Compositions of Examples I to IV
- the amount of the multi-site cation Sc was chosen as 0.25% with respect to the sum of cations in the formula unit of the stoichiometric garnet composition.
- the term "rel. density” means that the two most dense ceramics (which had the identical density) were arbitrarily set to have a relative density of 100%. It can be seen that all ceramics essentially have the same density. COMPARATIVE EXAMPLES I to IV Together with the inventive Examples, also four comparative Examples were made exactly as described above, only without at least one multisite element (i.e. no Sc).
- Table II shows the material compositions of the four inventive Examples I to IV: Table II: Compositions of ceramic YAG:Ce samples
- the term "rel. density” means here, too, that the densest ceramic was arbitrarily set to have a relative density of 100%. It can be seen that the deviation in density is a bit greater than in Table I and thus a large scatter in optical properties, e.g. scattering can be observed.
- Figs. 1 to 8 show the microstructures (SEM micrographs) of inventive Examples I to IV (Figs. 1 to 4 respectively) and comparative Examples I to IV (Figs. 5 to 8 respectively).
- Example II Although in the initial material mixture the Al-content was a bit to low. Due to the milling with alumina, some minute abrasion occurs, thereby slightly increasing the Al- content. Examples III and IV show both alumina second phase grains (visible as black grains in the scanning electron microscope image) that act as scattering centres in the ceramic.
- the comparative Example II is the least dense ceramic due to remaining internal porosity. It has been shown in a wide range of applications that without at least one multi-site element the materials with the exact composition are often the materials hardest to sinter, most likely because of a missing eutectic second phase that acts as a sintering aid. If a at least one multi-site element is added, this can be overcome; all inventive Examples showed excellent sintering properties
- the particular combinations of elements and features in the above detailed embodiments are exemplary only; the interchanging and substitution of these teachings with other teachings in this and the patents/applications incorporated by reference are also expressly contemplated.
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Abstract
The invention relates to a YAG-based ceramic garnet material comprising at least one multi-site element capable of replacing the Y and/or Al-sites within the YAG-material.
Description
YAG-BASED CERAMIC GARNET MATERIAL COMPRISING AT LEAST ONE MULTI-SITE ELEMENT
The present invention is directed to ceramic garnet materials, especially those materials which are of use in the context of light emitting devices, especially of LEDs.
Today's light emitting devices, especially LEDs comprise to a large extent Ce(III) doped YAG-based materials due to the excellent material properties of YAG. In this regard, it is e.g. referred to the US 2003 /0078156 Al which is hereby incorporated by reference. However, especially for light emitting devices which use Ce(III) doped
YAG-based materials in ceramic and/or crystalline form, it has been shown that the manufacture of those YAG-ceramics is often involved with difficulties, since especially the material composition must be kept exactly in order to avoid the presence of secondary phases, especially YAP (perovskite)-Phases in the YAG. Phase relations in the alumina - yttria system are known from e.g. J. S.
Abell, LR. Harris, B. Cockayne and B. Lent, J. Mater. Sci, 9 (1974) 527. In the solid state Y3AI5O12 (YAG) crystallizes as a line compound with either alumina, AI2O3, or YAP, YAIO3, as neighboring phases that are formed in poly crystalline garnet YAG materials, if deviations from ideal stoichiometry occur. From M. M. Kuklja and R. Pandey, J. Am. Ceram. Soc. 82 (1999) 2881, it is known, that intrinsic anti-site disorder is the dominant mechanism of accommodating for deviations from ideal stoichiometry, viz. an excess of Y2O3 or AI2O3, in Y3AI5O12 (YAG) garnet compound. Such anti-site disorder may lead to an extension of the single phase existence area surrounding the line compound stoichiometry
especially for compositions showing an yttria excess because incorporation of yttrium at octahedral aluminum sites is energetically more favorable than incorporation of aluminium at dodecahedral yttrium sites.
However, especially in the context of an industrial production of Ce(III) doped YAG-ceramics, it is often impossible to exactly keep the right composition due to weighing errors or fluctuations during the manufacturing process.
It is an object of the present invention to provide a YAG-based ceramic garnet material with improved properties which especially allows for a wide range of applications a greater production tolerance
This object is solved by a YAG-based ceramic garnet material according to claim 1 of thepresent invention and/or by a method according to claim9 of the present application. Accordingly, a YAG-based ceramic garnet material is provided comprising at least one multi-site element capable of occupying the octahedral and/or the dodecahedral coordinated cation lattice sites inside the YAG-based ceramic garnet material.
It has been surprisingly found out that by using such a YAG-based ceramic garnet material, in most applications within the present invention, the production tolerance can be greatly enhanced without affecting the features of the YAG-based ceramic. In some applications, the features of the YAG-based ceramic garnet material can even be improved. Without being determined to a certain theory, it is believed by the inventors that the ability of the at least one multi-site element to act as a placeholder for the other ions, especially the Y and/or Al ions in the YAG-material, helps to widen the processing window of the YAG-material.
The term "YAG-based" especially means and/or includes a material which comprises as a main constituent a material M^M^M^X^ with M1 selected out of the group Mg, Ca, Y, Na, Sr, Gd, La, Ce, Pr, Nd, Sm, Eu, Dy, Tb, Ho, Er, Tm, Yb, Lu or mixtures thereof, Mπ selected out of the group Al, Ga, Mg, Zn, Y, Ge, Sc, Zr, Ti, Hf, Lu or mixtures thereof, Mm selected out of the group Al, Si, B, Ge, Ga, V, As, Zn or mixtures thereof, X selected out of the group O, S, N, F, Cl, Br, I, OH and mixtures
thereof and built of M11X6 octahedra and M111X4 tetrahedra in which each octahedron is joint to six others through vertex-sharing tetrahedra. Each tetrahedron shares its vertices with four octahedra, so that the composition of the framework is (M11Xs)2(M111X2)S. Larger ions M1 occupy positions of 8-coordination (dodecahedral) in the interstices of the framework, giving the final composition M^M^M^X^ or M^M^M11^^.
The term "main constituent" means especially that > 95 %, preferably > 97 % and most preferred > 99 % of the YAG-based ceramic garnet material - without the at least one multisite element and possibly added dopant materials - consists out of this material. It should be noted that in some garnet materials within the present invention, the Mπ and Mm positions are at least partly occupied by atoms of the same element.
It should be noted that the YAG-based ceramic material may be doped with a material selected out of the group Lu, Pr, Sm, Tb, Dy, Ho, Er, Tm, Yb, La, Ce or mixtures thereof.
The term "YAG-based ceramic garnet material" in the sense of the present invention furthermore means and/or includes especially a mixture of the material as described above with additives which may be added during ceramic processing. These additives may be incorporated fully or in part into the final material, which then may also be a composite of several chemically different species and particularly include such species known to the art as fluxes. Suitable fluxes include alkaline earth - or alkaline - metal oxides and halides, borates, SiO2 and the like.
The term "ceramic material" in the sense of the present invention means and/or includes especially a crystalline or polycrystalline compact material or composite material with a controlled amount of pores or which is pore free.
The term "polycrystalline material" in the sense of the present invention means and/or includes especially a material with a volume density larger than 90 percent of the main constituent, consisting of more than 80 percent of single crystal domains, with each domain being larger than 0.5 μm in diameter and may have different crystallo graphic orientations. The single crystal domains may be connected by amorphous or glassy material or by additional crystalline constituents.
According to a preferred embodiment of the present invention, the ionic radius for six fold coordination of the at least one multi-site element is > 70 pm to < 104 pm and/or the ionic radius for eight fold coordination of the at least one multi-site element is > 85 pm to < 116 pm. This has been shown in many applications within the present invention to be most efficient.
It should be noted that in case several different multi-site elements are present it is especially preferred that all multi-site elements have an ionic radius as described; this goes mutatis mutandis for all other embodiments within the present invention. According to a preferred embodiment of the present invention, the ionic radius for six- fold coordination of the at least one multi-site element is > 75 pm to < 104 pm, more preferred > 88 pm to < 102 pm.
According to a preferred embodiment of the present invention, the ionic radius for eight-fold coordination of the at least one multi-site element is > 90 pm to < 114 pm, more preferred > 92 pm to < 112 pm.
According to one embodiment of the present invention, the concentration of the at least one multi-site element is > 0,5 mol% to < 5 mol% with respect to the YAG-based garnet structure. This has been shown to be the best suitable range in order to obtain the widest processing window without deteriorating the features of the YAG- material within a wide range of applications within the present invention.
According to one embodiment of the present invention, the concentration of the at least one multi-site element is > 0.1 atom% to < 0.7 atom%, preferably > 0.2 atom% to < 0.4 atom%, with respect to the sum of cations in the formula unit.
According to one embodiment of the present invention, the quotient of the sum of (Y, Lu, Gd, Pr, Sm, Tb, Dy, Ho, Er, Tm, Yb, La, Ce, Ca) and the sum of (Al, B, Si, Mg, Ge, Zr, Hf, Ga, Sc) in the ceramic garnet material is >0.590 to <0.610. By doing so, for a wide range of applications the most suitable YAG-ceramic materials can be obtained. Preferably is the quotient of the sum of (Y, Lu, Gd, Pr, Sm, Tb, Dy, Ho, Er, Tm, Yb, La, Ce, Ca) and the sum of (Al, B, Si, Mg, Ge, Zr, Hf) in the ceramic garnet material >0.593 to <0.607, more preferred >0.595 to <0.605.
According to a preferred embodiment of the present invention, the ratio
of the main phase towards possible secondary phase(s) in the YAG-based ceramic garnet material is >10 :1, preferably >20 :1 and most preferred >40 :1
The term "secondary phase" in the sense of the present invention especially means and/or includes a minor constituent of the final mixture exhibiting different chemical composition and/or crystal structure.
According to a preferred embodiment of the present invention, the at least one multi-site element is selected out of the group comprising Sc, Ga, Yb, Lu, Mg and mixtures thereof. These materials have proven themselves in practice in many applications. According to a preferred embodiment of the present invention, the photothermal stability of the Ce(III) doped YAG-based ceramic garnet material is >80% to <100% after exposure of the ceramic material for 1000 hrs at 2000C with a light power density of 10W/cm2 and an average photon energy of 2.75 eV.
The term "photothermal stability" in the sense of the present invention especially means and/or includes the conservation of the luminescence intensity under simultaneous application of heat and high intensity excitation, i.e. a photothermal stability of 100% indicates that the material is virtually unaffected by the simultaneous irradiation and heat up.
According to a preferred embodiment of the present invention, the photothermal stability of the Ce(III) doped YAG-based ceramic garnet material is
>82.5% to <95%, preferably >85% to <97%, after exposure of the ceramic material for 1000 hrs at 2000C with a light power density of 10W/cm2 and an average photon energy of 2.75 eV.
According to a preferred embodiment of the present invention, the thermal conductivity of the YAG-based ceramic garnet material is > 0.07 W Cm 1K"1 to < 0.15 W Cm 1K"1
According to a preferred embodiment of the present invention, the quantum yield of a Ce(III) doped YAG[PSi]-based ceramic garnet material is > 90% to < 99% The term "quantum yield" in the sense of the present invention especially means and/or includes the ratio of the number of photons emitted to the number of
photons absorbed.
According to a preferred embodiment of the present invention, the quantum yield of the YAG-based ceramic garnet material is > 93% to < 99%, preferably > 95% to < 98% According to one embodiment of the present invention, the YAG-based ceramic garnet material shows a transparency for normal incidence in air of >10 % to <85 % for light in the wavelength range from > 550 nm to < 1000 nm.
Preferably, the transparency for normal incidence is in air of >20 % to < 80 % for light in the wavelength range from > 550 nm to < 1000 nm, more preferred >30 % to <75 % and most preferred > 40% to < 70% for a light in the wavelength range from > 550 nm to < 1000 nm.
The term "transparency" in the sense of the present invention means especially that > 10% preferably >20%, more preferred >30%, most preferred >40% and <85% of the incident light of a wavelength, which cannot be absorbed by the material, is transmitted through the sample for normal incidence in air (at an arbitrary angle). This wavelength is preferably in the range of > 550 nm and <1000 nm.
According to a preferred embodiment of the present invention, the YAG- based ceramic garnet material has a density of >95% and < 101% of the theoretical density of the stoichiometric garnet structure. According to a preferred embodiment of the present invention, the YAG- based ceramic garnet material has a density of >97% and < 100% of the theoretical density.
The densities lower than 100% according to the described preferred embodiment of the present invention are preferably obtained by sintering of the ceramic to a stage where still pores are present in the ceramic matrix. Most preferred are densities in the range >98.0% and <99.8% with total pore volumes in the ceramic matrix within the >0.2 - <2% range. A preferred mean pore diameter is in the >400 - < 1500 nm range. The present invention furthermore relates to a method of producing a
YAG-based ceramic garnet material according to the present invention comprising a
sintering step.
The term "sintering step" in the sense of the present invention means especially densifϊcation of a precursor powder under the influence of heat, which may be combined with the application of uniaxial or isostatic pressure, without reaching the liquid state of the main constituents of the sintered material.
According to a preferred embodiment of the present invention, the sintering step is pressureless, preferably in reducing or inert atmosphere.
According to a preferred embodiment of the present invention, the method furthermore comprises the step of pressing the ceramic garnet precursor material to >50% to < 70 %, preferably >55% to < 65 %, of its theoretical density before sintering. It has been shown in practice that this improves the sintering steps for most YAG-based ceramic garnet materials as described with the present invention.
According to a preferred embodiment of the present invention, the method of producing a YAG-based ceramic garnet material according to the present invention comprises the following steps:
(a) Mixing the precursor materials for the YAG-based ceramic garnet material
(b) optional firing of the precursor materials, preferably at a temperature of >1300 0C to < 17000C to remove volatile materials (such as CO2 in case carbonates are used)
(c) optional grinding and washing
(d) a first pressing step, preferably a unixial pressing step using a suitable powder compacting tool with a mould in the desired shape (e.g. rod- or pellet- shape) and/ or a cold isostatic pressing step preferably at >3000 bar to < 5000 bar.
(e) a sintering step at >1500 0C to < 22000C in an inert ,reducing or slightly oxidizing atmosphere with a pressure of > 10~7mbar to < 104 mbar.
(f) an optional hot pressing step, preferably a hot isostatic pressing step preferably at >30 bar to < 2500 bar and preferably at a temperature of >1500 0C to < 20000C and/or a hot uniaxial pressing step preferably at >100 bar to < 2500 bar and preferably at a temperature of >1500 0C to < 20000C.
(g) optionally a post annealing step at >1000°C to < 17000C in inert atmosphere or in an oxygen containing atmosphere.
According to this method, for most desired material compositions this production method has produced the best YAG-based ceramic garnet materials as used in the present invention.
The present invention also relates to a light emitting device, especially a LED comprising a YAG-based ceramic garnet material of the present invention.
A YAG-based ceramic garnet material according to the present invention, a light emitting device comprising a YAG-based ceramic garnet material according to the present invention and/or a YAG-based ceramic garnet material as produced with the present method may be of use in a broad variety of systems and/or applications, amongst them one or more of the following:
Office lighting systems household application systems - shop lighting systems, home lighting systems, accent lighting systems, spot lighting systems, theatre lighting systems, - fiber-optics application systems, projection systems, self-lit display systems, pixelated display systems, segmented display systems, - warning sign systems, medical lighting application systems, indicator sign systems, and decorative lighting systems portable systems - automotive applications green house lighting systems
window materials and window applications laser applications systems, especially for polycrystalline laser materials with garnet host lattice light emitting device housings, especially for HID lamps - optical lenses or elements with high refractive index
The aforementioned components, as well as the claimed components and the components to be used in accordance with the invention in the described embodiments, are not subject to any special exceptions with respect to their size, shape, material selection and technical concept such that the selection criteria known in the pertinent field can be applied without limitations.
Additional details, features, characteristics and advantages of the object of the invention are disclosed in the dependent claims, the figures and the following description of the respective figures and examples, which —in an exemplary fashion- show several embodiments and examples of a YAG-based ceramic garnet material according to the invention.
Fig. 1 shows a microstructure of a YAG-based ceramic garnet material according to Example I of the present invention Fig. 2 shows a microstructure of a YAG-based ceramic garnet material according to Example II of the present invention
Fig. 3 shows a microstructure of a YAG-based ceramic garnet material according to Example III of the present invention
Fig.4 shows a microstructure of a YAG-based ceramic garnet material according to Example IV of the present invention
Fig. 5 shows a microstructure of a YAG ceramic garnet material according to Comparative Example I
Fig. 6 shows a microstructure of a YAG ceramic garnet material according to Comparative Example II Fig. 7 shows a microstructure of a YAG ceramic garnet material according to Comparative Example III.
Fig. 8 shows a microstructure of a YAG ceramic garnet material according to Comparative Example IV
EXAMPLES I to IV
The invention will be better understood together with the Examples I to IV which - in a mere illustrative fashion - are four Examples of inventive YAG-based ceramic garnet materials.
The garnet materials were made the following way: First, the appropriate amounts of powders of Y2O3 (99.99%, Rhodia),
Gd2O3 (99.99%, Rhodia), Sc2O3 (99.9%) , Al2O3 (99,99%, Baikowski) and CeO2 (> 99%, Rhodia) were weighed in and milling with high density alumina milling media in isopropanol with 1000 ppm silica added as hydro lyzed tetraethoxysilane was carried out. Afterwards, the ceramic slurry was sieved to remove coarser particles and dried after addition of a polyvinylbutyral based binder system. The powder mixture was then granulated and ceramic green bodies were formed by means of cold isostatic pressing. After removing the binder in air atmosphere, the ceramic green bodies are sintered at temperatures in the range 1600 - 17500C in a H2/N2 (5%/95%) atmosphere. After machining, the ceramic parts were postannealed at 12000C - 14000C in air atmosphere. Table I shows the material compositions of the four inventive Examples I to IV: Table 1 : Compositions of Examples I to IV
The amount of the multi-site cation Sc was chosen as 0.25% with respect to the sum of cations in the formula unit of the stoichiometric garnet composition.
The term "rel. density" means that the two most dense ceramics (which had the identical density) were arbitrarily set to have a relative density of 100%. It can be seen that all ceramics essentially have the same density. COMPARATIVE EXAMPLES I to IV Together with the inventive Examples, also four comparative Examples were made exactly as described above, only without at least one multisite element (i.e. no Sc).
Table II shows the material compositions of the four inventive Examples I to IV: Table II: Compositions of ceramic YAG:Ce samples
The term "rel. density" means here, too, that the densest ceramic was arbitrarily set to have a relative density of 100%. It can be seen that the deviation in density is a bit greater than in Table I and thus a large scatter in optical properties, e.g. scattering can be observed.
Figs. 1 to 8 show the microstructures (SEM micrographs) of inventive Examples I to IV (Figs. 1 to 4 respectively) and comparative Examples I to IV (Figs. 5 to 8 respectively).
It can be seen that all inventive Examples show an uniform structure with no secondary phase to be seen, whereas in all comparative Examples secondary phases are present.
It should be shortly noted that the best comparative Example is Example II, although in the initial material mixture the Al-content was a bit to low. Due to the milling with alumina, some minute abrasion occurs, thereby slightly increasing the Al- content. Examples III and IV show both alumina second phase grains (visible as
black grains in the scanning electron microscope image) that act as scattering centres in the ceramic.
However, it is apparent that the comparative Example II is the least dense ceramic due to remaining internal porosity. It has been shown in a wide range of applications that without at least one multi-site element the materials with the exact composition are often the materials hardest to sinter, most likely because of a missing eutectic second phase that acts as a sintering aid. If a at least one multi-site element is added, this can be overcome; all inventive Examples showed excellent sintering properties The particular combinations of elements and features in the above detailed embodiments are exemplary only; the interchanging and substitution of these teachings with other teachings in this and the patents/applications incorporated by reference are also expressly contemplated. As those skilled in the art will recognize, variations, modifications, and other implementations of what is described herein can occur to those of ordinary skill in the art without departing from the spirit and the scope of the invention as claimed. Accordingly, the foregoing description is by way of example only and is not intended as limiting. The invention's scope is defined in the following claims and the equivalents thereto. Furthermore, reference signs used in the description and claims do not limit the scope of the invention as claimed.
Claims
1. A YAG-based ceramic garnet material comprising a at least one multi-site element capable of occupying the octahedral and/or the dodecahedral sites inside the YAG-based ceramic garnet material
2. The YAG-based ceramic garnet material of claim 1 , whereby the ionic radius of the at least one multi-site element on the six fold coordinated cation lattice site that is incorporated into the Ce(III) doped YAG-based ceramic garnet material is > 70 pm to < 104 pm
3. The YAG-based ceramic garnet material of claim 1 or 2, whereby the concentration of the at least one multi-site element is > 0,1 atom% to < 0.7 atom% of the sum of cations of the garnet structure.
4. The YAG-based ceramic garnet material of any of the claims 1 to 3 whereby the quotient of the sum of (Y, Lu, Gd, Pr, Sm, Tb, Dy, Ho, Er, Tm, Yb, La,
Ce, Ca) and the sum of (Sc, Ga, Al, B, Mg, Si, Ge, Zr, Hf) in the ceramic garnet material is >0.590 to <0.610.
5. The YAG-based ceramic garnet material of any of the claims 1 to 4 whereby the ratio of the main phase towards possible secondary phase(s) in the
YAG-based ceramic garnet material with is > 10 : 1
6. The YAG-based ceramic garnet material of any of the claims 1 to 5 whereby the at least one multi-site element is selected out of the group comprising Sc, Ga, Yb, Lu, Mg and mixtures thereof
7. The YAG-based ceramic garnet material of any of the claims 1 to 6 whereby the photothermal stability of the YAG-based ceramic garnet material is is >80% to <100% after exposure of the ceramic material for 1000 hrs at 2000C with a light power density of 10W/cm2 and an average photon energy of 2.75 eV.
8. A light-emitting device, especially a LED comprising a YAG-based ceramic garnet material of any of the claims 1 to 7.
9. A method of producing a YAG-based ceramic garnet material for a light- emitting device according to any of the claims 1 to 7 comprising a sintering step.
10. A system comprising a a YAG-based ceramic garnet material according to any of the claims 1 to 7, a light emitting device according to claim 8 and/or a YAG-based ceramic garnet material as produced according to the method of the claims 9, the system being used in one or more of the following applications:
Office lighting systems household application systems shop lighting systems, - home lighting systems, accent lighting systems, spot lighting systems, theatre lighting systems, fiber-optics application systems, - projection systems, self-lit display systems, pixelated display systems, segmented display systems, warning sign systems, - medical lighting application systems, indicator sign systems, and decorative lighting systems portable systems automotive applications - green house lighting systems window materials and window applications laser applications systems, especially for polycrystalline laser materials with garnet host lattice light emitting device housings, especially for HID lamps - optical lenses or elements with high refractive index.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP07805095A EP2049450A1 (en) | 2006-07-26 | 2007-07-10 | Yag-based ceramic garnet material comprising at least one multi-site element |
| JP2009521389A JP2009544791A (en) | 2006-07-26 | 2007-07-10 | YAG-based ceramic garnet material containing at least one multisite element |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP06117845 | 2006-07-26 | ||
| EP06117845.5 | 2006-07-26 |
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| WO2008012712A1 true WO2008012712A1 (en) | 2008-01-31 |
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|---|---|---|---|
| PCT/IB2007/052725 WO2008012712A1 (en) | 2006-07-26 | 2007-07-10 | Yag-based ceramic garnet material comprising at least one multi-site element |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP2049450A1 (en) |
| JP (1) | JP2009544791A (en) |
| KR (1) | KR20090040450A (en) |
| CN (1) | CN101495424A (en) |
| RU (1) | RU2009106671A (en) |
| TW (1) | TW200811078A (en) |
| WO (1) | WO2008012712A1 (en) |
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Also Published As
| Publication number | Publication date |
|---|---|
| TW200811078A (en) | 2008-03-01 |
| JP2009544791A (en) | 2009-12-17 |
| RU2009106671A (en) | 2010-09-10 |
| CN101495424A (en) | 2009-07-29 |
| KR20090040450A (en) | 2009-04-24 |
| EP2049450A1 (en) | 2009-04-22 |
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