CN103881710B - 荧光体与发光装置 - Google Patents
荧光体与发光装置 Download PDFInfo
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- CN103881710B CN103881710B CN201310130888.6A CN201310130888A CN103881710B CN 103881710 B CN103881710 B CN 103881710B CN 201310130888 A CN201310130888 A CN 201310130888A CN 103881710 B CN103881710 B CN 103881710B
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 20
- 239000011733 molybdenum Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000011575 calcium Substances 0.000 claims abstract description 16
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 11
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052788 barium Inorganic materials 0.000 claims abstract description 8
- 239000011777 magnesium Substances 0.000 claims abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 4
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 239000004065 semiconductor Substances 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 7
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 26
- 239000002245 particle Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 18
- 239000002994 raw material Substances 0.000 description 18
- 238000005245 sintering Methods 0.000 description 17
- 238000000034 method Methods 0.000 description 15
- 239000013078 crystal Substances 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- 230000000977 initiatory effect Effects 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 8
- 150000004767 nitrides Chemical class 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 229910052581 Si3N4 Inorganic materials 0.000 description 7
- -1 nitrogen-containing compound Chemical class 0.000 description 6
- 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 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000004020 luminiscence type Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052582 BN Inorganic materials 0.000 description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002601 GaN Inorganic materials 0.000 description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910001940 europium oxide Inorganic materials 0.000 description 3
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 3
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052571 earthenware Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- STZJANGYOWJEPH-UHFFFAOYSA-N carbonic acid;molybdenum Chemical compound [Mo].OC(O)=O STZJANGYOWJEPH-UHFFFAOYSA-N 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/0883—Arsenides; Nitrides; Phosphides
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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
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
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- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/481—Disposition
- H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/48245—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
- H01L2224/48247—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic connecting the wire to a bond pad of the item
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- H01L2224/85—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a wire connector
- H01L2224/85909—Post-treatment of the connector or wire bonding area
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Abstract
本发明提供一种荧光体发光装置。该荧光体包括组成式为AaSi5OtNn:EuZ的组合物,其中A元素选自铍(Be)、镁(Mg)、钙(Ca)、锶(Sr)及钡(Ba)元素;1.7<a<2.5;0≦t<1;7<n<9;0.001<z<0.3。所述荧光体具有10ppm~500ppm的钼(Mo)。
Description
【技术领域】
本发明涉及一种荧光体与使用其的发光装置,且特别是涉及一种组成式为AaSi5OtNn:EuZ的荧光体与使用其的发光装置。
【背景技术】
近年,使用半导体发光的发光装置被广泛地使用,特别是发光二极管已被成功开发,此发光装置较现有的冷阴极灯管、白炽灯等发光设备,具有发光效率高、体积小、低耗电力与低成本等优点,因此可作为各种光源来使用。而半导体发光装置包含半导体发光元件与荧光体,荧光体可吸收并转换半导体发光元件所发出的光,由此半导体发光元件所发出的光与荧光体转换发出的光两者混合使用。此种发光装置可作为荧光灯、车辆照明、显示器、液晶背光显示等各种领域使用,其中,以白色发光装置使用最为广泛。现行白色发光装置是采用铈为活性中心的YAG荧光体(Y3Al5O12:Ce)并搭配发出蓝光的半导体发光元件所组成。然而,使用Y3Al5O12:Ce荧光体并搭配发出蓝光的半导体发光元件所发出的混合光,其色度座标位于发出蓝光的半导体发光元件的色座标与Y3Al5O12:Ce荧光体的色座标连接线上,因而,所发出的混合光为缺乏红色光的白光,演色性与色彩饱和度明显不足。此外,Y3Al5O12:Ce的较佳激发光谱区域和半导体发光元件的发光区域并不一致,因此,激发光的转换效率不佳,高辉度的白光光源不易获得。为解决此种色调不良和发光辉度低下的现象,近年积极开发将YAG:Ce荧光体中混入可发出红光的荧光体,并改良可发出红光的荧光体的品质,以提高发光辉度。
然而,吸收蓝色光进而发出红色光的荧光体较为稀少,目前业界的开发研究以氮化物、氮氧化物荧光体为主。已知有使用铕(Eu)为活性中心的Sr2Si5N8:Eu荧光体、CaAlSiN3:Eu荧光体及一般式为MzSi12-(m+n)Alm+nOnN16-n:Eu的赛隆荧光体。然而,Sr2Si5N8:Eu荧光体由于发光辉度不佳,应用性受到局限,近年使用上并不普及;赛隆荧光体本身无耐久性问题,但是荧光体发光辉度明显不足,商业使用上并不普及。CaAlSiN3:Eu荧光体虽然有较佳的耐久性,以及比赛隆荧光体佳的辉度,但业界仍期待能更进一步提高荧光体的发光辉度,以使发光装置能具有较高的发光效率。
【发明内容】
鉴于上述问题,因此本发明的目的在于提供高辉度的荧光体材料,以及提供使用所述的荧光体材料搭配半导体发光元件而构成一高辉度的发光装置。
根据实施例,提供一种荧光体。荧光体包括组成式为AaSi5OtNn:EuZ的组合物。A元素选自由铍(Be)、镁(Mg)、钙(Ca)、锶(Sr)及钡(Ba)元素。1.7<a<2.5。0≦t<1。7<n<9。0.001<z<0.3。荧光体具有10ppm~500ppm的钼(Mo)。
根据实施例,提供一种发光装置。发光装置包括半导体发光元件与上述荧光体。荧光体受半导体发光元件所发出的光激发,并转换发出波长相异于半导体发光元件所发出光的光。
【附图说明】
图1是本发明发光装置实施例的透视图。
【主要附图标记说明】
21~半导体发光元件;
22~荧光层;
23~封装层;
211~基座;
212~承载面;
213~发光二极管晶粒;
214~连接线;
215~导线;
221~荧光体。
【具体实施方式】
在实施例中,荧光体包括组成式为AaSi5OtNn:EuZ的组合物,并且荧光体具有钼(Mo)元素。添加钼后的荧光体,相比于色度相同下的未添加钼的荧光体具有较高的辉度值。所谓色度相同意味着色度座标x、y差异分别在±0.002之内。
在实施例中,A元素选自铍(Be)、镁(Mg)、钙(Ca)、锶(Sr)及钡(Ba)元素。A元素优选选自钙(Ca)、锶(Sr)及钡(Ba)元素。1.7<a<2.5,优选为1.8<a<2.3。0≦t<1,优选为0≦t<0.5。7<n<9,优选为7<n<8。
此外,荧光体中含有的钼含量,对于荧光体的发光辉度有所影响,因此需通过控制钼的含量在特定范围,达到高发光辉度的效果。本发明的荧光体具有钼(Mo)元素10ppm~500ppm,过多或过少的钼都会使得辉度下降。在实施例中,荧光体具有钼元素优选为20ppm~350ppm,更优选为25ppm~200ppm。
荧光体中,0.001<z<0.3。若荧光体的发光中心的Eu数量过少,会使得荧光体的发光辉度降低。若荧光体的发光中心的Eu数量过高,由于Eu原子间的相互干扰而造成浓度消光的现象,以致辉度减低。优选地,当0.01<z<0.05时,发光辉度更佳。
当使用455nm光源照射本发明的荧光体时,荧光体受激发而发出的发光主波长为580nm~680nm,其发光色调的CIE1931色度座标(x,y)为0.45≦x≦0.72,0.2≦y≦0.5。发光主波长是指发光光谱中发光强度最大的波长。
本发明的荧光体制造时,硅元素的原料可使用含氮化合物、含氧化合物、任何形式的化合物或硅的元素态。例如,可混合使用硅元素的氮化物(Si3N4)/氧化物(SiOx)。所谓「含氧化合物」可包含氧化物、碳酸盐、草酸盐等化合物。含氮化合物的情况,亦是指具有硅元素与氮的化合物。
欲达到本发明的钼的含量范围,优选可通过外添加方式烧结实施。添加的钼的前驱物并无特别限制,可为钼金属、碳酸钼、氮化钼、氧化钼、氢氧化钼、氢化钼等各种实施样态。其中以氧化钼的实施效果较佳。例如三氧化钼、二氧化钼等的氧化钼,其中尤以三氧化钼效果最佳。
本发明荧光体原料可为各种不同形式的前驱物,为方便起见以下以氮化物与氧化物原料作为实施方式说明。A元素与Si元素的氧化物或氮化物原料虽可为市售原料,但是因为纯度越高越好,因此最好准备3N(99.9%)以上的原料为佳。各原料粒子的粒径从促进反应的观点而言,最好为微粒子,但是随原料的粒径、形状不同,所获得荧光体的粒径、形状亦将有所变化。因此只要配合最终所获得荧光体要求的粒径,准备具有近似粒径的氮化物、氧化物原料即可。Eu元素的原料以市售氧化物、氮化物原料或金属为佳,纯度越高越好,最好准备2N(99%)以上,尤以3N(99.9%)以上的原料为佳。
原料的混合方式,可为干式法、湿式法。例如干式球磨法或加入液体的湿式球磨法等多种实施方式,并不局限于单一方式。称取、混合Ca3N2、Sr3N2、Si3N4、Ba3N2时,因为这些化合物较易被氧化,因而在非活性环境下的手套箱内进行操作较为适当。此外,因为各原料元素的氮化物较容易受水分的影响,因此,用于充填手套箱的非活性气体最好使用经充分去除水分的气体。此外,若为湿式混合法,当所使用的液体为纯水时,原料将遭分解,因此,必须选择适当的有机溶剂。混合装置可使用球磨机或研钵等通常所使用的装置。
制备荧光体时可依一定比例称量、混合各原料,置入坩埚中,再置入高温炉中烧结。烧结时使用的高温炉,因烧结温度为高温,故优选为使用金属电阻加热方式或石墨电阻加热方式的高温炉。作为烧结方法,优选的是常压烧结法或气压(以气体加压)烧结法等外部未施加机械性加压的烧结方法。坩锅优选为不纯物含量极低的高纯度材质,如Al2O3坩锅、Si3N4坩锅、AlN坩锅、赛隆坩锅、BN(氮化硼)坩锅等可在非活性环境中使用的坩锅,其中以使用BN坩锅为最佳,因其对于避免源自坩锅的不纯物混入的效果最佳。烧结气氛为非氧化性气体,例如,可为氮、氢、氨、氩等或前述气体的任意组合。荧光体的烧结温度为1200℃以上、2200℃以下,更优选为1400℃以上、2000℃以下,升温速度为3~15℃/min。较低温下烧结可得较细微荧光体,较高温下烧结可得粒径较大荧光体。烧结时间根据原料种类不同而有所差异,一般反应时间为1~12小时较佳。烧结时在非活性环境下的压力,例如是在0.5MPa以下(尤以0.1MPa以下为佳)进行烧结。烧结完成后,冷却至室温,可使用球磨、或工业用粉碎机械等方式粉碎,再经过水洗、过滤、干燥、分级等步骤,即可得到本发明的荧光体。
为了获得高辉度的荧光体,荧光体于烧结时,因助熔剂的添加、原料中的杂质、处理过程污染等因素的影响,包含在所述荧光体组成中的杂质含量应尽可能小。特别是氟元素、硼元素、氯元素、碳元素等元素大量存在时,将抑制发光。因此可选择较高纯度的原料,和控制合成步骤避免污染,使得前述氟、硼、氯、碳等元素的含量分别小于1000ppm。
当本发明的荧光体以粉体的形式使用时,荧光体粉体的平均粒径最好在30μm以下。理由是因为荧光体粉体的发光主要是发生于粒子表面上,若平均粒径(本发明中所谓的「平均粒径」是指体积中值粒径(D50))在30μm以下,将可确保粉体每单位重量的表面积,避免辉度降低。此外,将粉体涂布于发光元件之上的情况,可提高粉体的密度,就此观点而言,亦可避免辉度降低。另外,从荧光体粉末的发光效率观点而言,平均粒径以大于1μm为较佳。依上述,本发明荧光体粉体的平均粒径最好在1μm以上且30μm以下,尤以3.0μm以上且20μm以下的粒径为佳。此处所谓的「平均粒径(D50)」,是利用Beckman Coulter公司制MultiSizer-3,以库尔特法(体积中值粒径D50)进行测定所得的值。
本发明的荧光体适用于荧光显示管(VFD)、场发射显示器(FED)、等离子体显示器(PDP)、阴极射线管(CRT)、发光二极管(LED)等。尤其是,本发明的荧光体当使用455nm光源照射时,发光主波长为580nm~680nm,发光色调的CIE1931色度座标(x,y)为,0.45≦x≦0.72,0.2≦y≦0.5,且发光辉度高,因此特别适用于发光二极管。
本发明的发光装置包含半导体发光元件及本发明的荧光体。半导体发光元件以发出波长为300~550nm的光的元件为较佳,尤其以发出330~420nm的紫外(或紫)光半导体发光元件或420~500nm的蓝色半导体发光元件较佳。作为这些发光元件,半导体发光元件可为硫化锌或氮化镓等各种半导体,而以发光效率而言,使用氮化镓半导体较佳。氮化镓发光元件可通过有机金属化学气相沉积法(MOCVD)或氢化物气相磊晶法(HVPE)等方法在基板上形成氮化物半导体,以InαAlβGa1-α-βN(0≦α、0≦β、α+β<1)所形成的半导体发光元件最佳。半导体构造可为MIS接合、PIN接合、PN接合等均质构造、异质接面构造或双异质接面构造。此外,可通过调整半导体层的材料或其混晶度来控制其发光波长。
本发明的发光装置中,除了将本发明的荧光体单独使用外,亦可与具有其他发光特性的荧光体一起使用,以构成可发出所想要的颜色的发光装置。例如,使用330~420nm的紫外光半导体发光元件搭配在此波长被激发而发出420nm以上且500nm以下波长的蓝色荧光体、发出500nm以上且570nm以下的波长之绿色荧光体、以及本发明荧光体的组合。前述蓝色荧光体举例可为BaMgAl10O17:Eu,绿色荧光体可为β-赛隆荧光体。依此构成,当半导体发光元件所发出的紫外线照射于荧光体时,会发出红、绿、蓝三色光,经由其混合而成为白色发光装置。
此外,还可使用420~500nm的蓝色半导体发光元件搭配在此波长被激发而发出550nm以上且600nm以下波长的黄色荧光体、以及本发明荧光体的组合。前述黄色荧光体,例如可为Y3Al5O12:Ce。依此构成,当半导体发光元件所发出的蓝色光照射于荧光体时,会发出红、黄之二色光,将这些光与半导体发光元件本身的蓝色光混合而成为白色或带灯泡色的照明器具。
此外,还可使用420~500nm的蓝色半导体发光元件搭配在此波长被激发而发出500nm以上且570nm以下波长的绿色荧光体、以及本发明荧光体的组合。此种绿色荧光体举例可为β-赛隆荧光体。依此构成,当半导体发光元件所发出的蓝色光照射于荧光体时,会发出红、绿之二色光,将这些光与半导体发光元件本身的蓝色光混合而成为白色照明器具。
[实施例及比较例]
以下,就本发明实施例加以说明,但是本发明并不仅限定于此。
测量方法:
(1)荧光体辉度及色度座标:荧光体以TOPCON辉度计SR-3A使用455nm照射测量。辉度值测量差异为±0.3%以内。
(2)荧光体发光主波长:以Jobin YVON的Fluoro Max-3进行测量。发光主波长是指使用455nm光激发荧光体时,荧光体最大发光强度的波长。
(3)荧光体组成元素的分析:
(3-1a)仪器:以Jobin YVON的ULTIMA-2型感应耦合等离子体原子放射光谱仪(ICP)进行元素含量的测量。
(3-1b)样品前处理:准确称取0.1g的样品,在白金坩锅内,加入Na2CO31g混合均匀后,以1200℃高温炉熔融(温度条件:由室温升温2小时到达1200℃,于1200℃恒温5小时),待熔融物冷却后加入酸溶液,例如25mlHCl(36%),并加热溶解至澄清,冷却后置入100ml PFA定量瓶中,以纯水定量至标线。
(3-2a)仪器:Horiba的氮氧分析仪。型号EMGA-620W。
(3-2b)测量:将荧光体20mg置入锡胶囊内,放置于坩埚中,进行测量。
合成例1
准备所需的钙金属(3N7,99.97%)、锶金属(4N,99.99%)和钡金属(2N,99%),粉碎后分别置于纯氮气氛下直接烧结形成氮化物,反应条件分别为750℃、700℃、700℃下烧结24小时。可分别获得氮化钙(Ca3N2)、氮化锶(Sr3N2)和氮化钡(Ba3N2)的化合物。
实施例1~实施例5、比较例1~比较例3
实施例1~实施例5、比较例1~比较例3的荧光体制造方式相同,差异主要在于三氧化钼(MoO3)的使用量不同,以下以实施例3为例说明荧光体的制造方法。
在实施例3中,称取204.648g合成例1合成的氮化锶(Sr3N2)化合物、250.000g氮化硅(Si3N4,纯度3N)及4.892g氧化铕(Eu2O3,纯度4N)、0.046g三氧化钼(MoO3,纯度2N)在氮气环境下于手套箱中使用研钵进行混合,形成荧光体起始原料,其中三氧化钼原料占荧光体起始原料(表1的Mo wt.%栏)0.003wt.%。
然后,将荧光体起始原料置入以氮化硼为材质的烧结容器中,接着将含有起始原料的烧结容器置入含有高纯度氮气的高温炉中,氮气气体流量为80升/分,依10℃/min的升温速度升温至1800°C,并在1800°C下保持8小时,且高温炉操作压力维持在0.1MPa,以进行烧结。烧结后,依10℃/min的降温速率降至室温,再经由粉碎、球磨、水洗二次、过滤、干燥及分级等步骤,即获得荧光体。
实施例3的氮氧分析仪及ICP分析结果为荧光体具有组成式Sr1.926Si5O0.108N7.416:Eu0.021,亦即,AaSi5OtNn:EuZ式中,A元素为Sr,a=1.926,t=0.108,n=7.416,z=0.021。荧光体的钼含量为87ppm。
实施例6
实施例6与实施例3的荧光体制造方式相同,差异主要在于三氧化钼(MoO3)改成使用二氧化钼(MoO2),其中二氧化钼原料占荧光体起始原料(表1的Mo wt.%栏)0.010wt.%。
实施例7
实施例7与实施例3的荧光体制造方式相同,差异主要在于实施例7的荧光体起始原料是称取90.846g合成例1合成的氮化锶(Sr3N2)化合物、137.423g合成例1合成的氮化钡(Ba3N2)化合物、224.000g的氮化硅(Si3N4,纯度3N)及7.418g氧化铕(Eu2O3,纯度4N)、0.046g三氧化钼(MoO3,纯度2N)在氮气环境下于手套箱中使用研钵进行混合,以形成荧光体起始原料,其中三氧化钼原料占荧光体起始原料(表1的Mo wt.%栏)0.010wt.%。
实施例8
实施例8与实施例3的荧光体制造方式相同,差异主要在于实施例8的荧光体起始原料是称取5.326g合成例1合成的氮化钙(Ca3N2)、193.954g合成例1合成的氮化锶(Sr3N2)化合物、252.000g氮化硅(Si3N4,纯度3N)及8.345g氧化铕(Eu2O3,纯度4N)、0.046g三氧化钼(MoO3,纯度2N)在氮气环境下于手套箱中使用研钵进行混合,形成荧光体起始原料。
表1列示各实施例与比较例的荧光体起始原料使用的钼来源化合物及其所占的重量比。此外,表1也列示得到的荧光体的性质,包括具有的A元素、组成(以基于组成式CaiSrjBakSi5OtNn:EuZ的原子数量表示,其中i、j、k的数目总和即为组成式AaSi5OtNn:EuZ中的a)、钼元素含量(Mo(ppm))、与色度座标x、y下的发光辉度。荧光体的发光光谱的主波长是指发光强度最大的波长。
表1
根据表1,在色度相同下,实施例1、2、6~8的辉度高于比较例1;在色度相同下,实施例3~5的辉度高于比较例2。
接着,将前述本发明各实施例的荧光体样品与半导体发光元件进行封装后制得本发明的发光装置。
参阅图1,本发明发光装置实施例包含半导体发光元件21、荧光层22及封装层23。
其中,半导体发光元件21包括可导电且具有一概呈凹型的承载面212的基座211、设置于凹型承载面212且与基座211电连接的发光二极管晶粒213、连接线214与发光二极管晶粒213电连接、导线215与连接线214电连接;其中,基座211与导线215可配合自外界提供电能至发光二极管晶粒213,发光二极管晶粒213可将接受的电能转换成光能向外发出。本实施例是将市售发光波长455nm,InGaN的蓝色发光二极管晶粒213(制造商:奇力光电)以导电银胶(型号:BQ6886,制造商:UNINWELL)黏合在基座211的承载面212上,接着自发光二极管晶粒213顶面延伸出与发光二极管晶粒213电连接的连接线214及导线215。
前述荧光层22包覆发光二极管晶粒213。荧光层22中所含的荧光体221在受到发光二极管晶粒213所发出的光的激发后,会转换发出异于激发光波长的光,在本实施例中,荧光层22是将含有35重量%荧光体221的聚硅烷氧树脂涂布在发光二极管晶粒213外表面,并经干燥硬化后而形成。
封装层23包覆半导体发光元件21部分的基座211、连接线214、部分的导线215及荧光层22。
综上所述,实施例的荧光体具有高辉度。且荧光体搭配半导体发光元件,可同时得到高辉度的发光装置。
Claims (7)
1.一种荧光体,其中该荧光体包括组成式为AaSi5OtNn:EuZ的组合物,该A元素选自由铍(Be)、镁(Mg)、钙(Ca)、锶(Sr)及钡(Ba)元素,1.7<a<2.5,0<t<1,7<n<9,0.001<z<0.3,该荧光体具有10ppm~92ppm的钼(Mo)。
2.如权利要求1所述的荧光体,其中该荧光体具有10ppm~87ppm的钼(Mo)。
3.如权利要求1所述的荧光体,其中该荧光体具有10ppm~28ppm的钼(Mo)。
4.如权利要求1所述的荧光体,其中1.8<a<2.3,0<t<0.5,7<n<8,0.01<z<0.05。
5.如权利要求1所述的荧光体,其中该A元素选自钙(Ca)、锶(Sr)及钡(Ba)元素。
6.如权利要求1所述的荧光体,其中使用455nm光源照射该荧光体,该荧光体受激发而发出发光主波长为580nm~680nm的光,其发光色调的CIE 1931色度座标(x,y)为0.45≦x≦0.72,0.2≦y≦0.5。
7.一种发光装置,包括:
半导体发光元件;以及
荧光体,包括如权利要求1至6中任一项所述的荧光体,其中该荧光体受该半导体发光元件所发出的光激发,并转换发出波长相异于该半导体发光元件所发出光的光。
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