TWI407474B - 陶瓷冷光轉換器及包含該轉換器之照明系統 - Google Patents
陶瓷冷光轉換器及包含該轉換器之照明系統 Download PDFInfo
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- TWI407474B TWI407474B TW095100773A TW95100773A TWI407474B TW I407474 B TWI407474 B TW I407474B TW 095100773 A TW095100773 A TW 095100773A TW 95100773 A TW95100773 A TW 95100773A TW I407474 B TWI407474 B TW I407474B
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- 238000004020 luminiscence type Methods 0.000 title claims abstract description 62
- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- 238000005286 illumination Methods 0.000 title claims abstract description 36
- 230000005855 radiation Effects 0.000 claims abstract description 50
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 31
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 16
- 229910052788 barium Inorganic materials 0.000 claims abstract description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 14
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 14
- 239000011575 calcium Substances 0.000 claims abstract description 14
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 17
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 14
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 14
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
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- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 3
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- MGVUQZZTJGLWJV-UHFFFAOYSA-N europium(2+) Chemical group [Eu+2] MGVUQZZTJGLWJV-UHFFFAOYSA-N 0.000 abstract 2
- 239000000843 powder Substances 0.000 description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
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- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000003595 spectral effect Effects 0.000 description 7
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- -1 aluminum-substituted cerium Chemical class 0.000 description 4
- 230000000295 complement effect Effects 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- SVJLBBSKJLMTRQ-UHFFFAOYSA-N ytterbium(2+) Chemical compound [Yb+2] SVJLBBSKJLMTRQ-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- KMKLUVYHNKQOSE-UHFFFAOYSA-N [Ce+2] Chemical compound [Ce+2] KMKLUVYHNKQOSE-UHFFFAOYSA-N 0.000 description 3
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- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- YAYGSLOSTXKUBW-UHFFFAOYSA-N ruthenium(2+) Chemical compound [Ru+2] YAYGSLOSTXKUBW-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- KAJPZYFHSCFBCI-UHFFFAOYSA-N yttrium(2+) Chemical group [Y+2] KAJPZYFHSCFBCI-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- BCZWPKDRLPGFFZ-UHFFFAOYSA-N azanylidynecerium Chemical compound [Ce]#N BCZWPKDRLPGFFZ-UHFFFAOYSA-N 0.000 description 2
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- JDBJCLFKHBHOBN-UHFFFAOYSA-N bismuth(2+) Chemical compound [Bi+2] JDBJCLFKHBHOBN-UHFFFAOYSA-N 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- DQUIAMCJEJUUJC-UHFFFAOYSA-N dibismuth;dioxido(oxo)silane Chemical compound [Bi+3].[Bi+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O DQUIAMCJEJUUJC-UHFFFAOYSA-N 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine group Chemical group NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
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- 238000005424 photoluminescence Methods 0.000 description 2
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- QSQXISIULMTHLV-UHFFFAOYSA-N strontium;dioxido(oxo)silane Chemical compound [Sr+2].[O-][Si]([O-])=O QSQXISIULMTHLV-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MCSXGCZMEPXKIW-UHFFFAOYSA-N 3-hydroxy-4-[(4-methyl-2-nitrophenyl)diazenyl]-N-(3-nitrophenyl)naphthalene-2-carboxamide Chemical compound Cc1ccc(N=Nc2c(O)c(cc3ccccc23)C(=O)Nc2cccc(c2)[N+]([O-])=O)c(c1)[N+]([O-])=O MCSXGCZMEPXKIW-UHFFFAOYSA-N 0.000 description 1
- 229910018509 Al—N Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910003849 O-Si Inorganic materials 0.000 description 1
- 229910003872 O—Si Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical class [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- YXJYBPXSEKMEEJ-UHFFFAOYSA-N phosphoric acid;sulfuric acid Chemical compound OP(O)(O)=O.OS(O)(=O)=O YXJYBPXSEKMEEJ-UHFFFAOYSA-N 0.000 description 1
- 210000004508 polar body Anatomy 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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Description
本發明大體上係關於一種包含一輻射源及一陶瓷冷光轉換器之照明系統。本發明亦關於一用於此種照明系統之陶瓷冷光轉換器。
更特定言之,本發明係關於一照明系統及一陶瓷冷光轉換器,該陶瓷冷光轉換器用於以一紫外光或藍光輻射發射輻射源為基礎,藉由發光下轉換加上色彩混合,來產生特定的有色光,包括白光。特別是針對以發光二極體作為輻射源的情況。
最近,在使用發光二極體作為輻射源來製造發射白光的照明系統方面,已有許多嘗試。當採用紅、綠及藍色發光二極體之配置來產生白光時,由於發光二極體之色調、光度及其他因素之變化,而無法產生所需色調之白光,這是一直都存在的問題。
為了解決這些問題,先前已有許多不同的照明系統被開發出來,這些系統利用含一磷光質的發光材料來轉換發光二極體所發射光線的顏色,以提供可見的白光照明。
先前的白光照明系統特別都是根據混合黃色和藍色的二色(BY)方法為主,這種方法中,輸出光線的黃色次要成分可以利用黃色磷光質提供,而藍色成分可利用磷光質或藍色LED的主要發射光線提供。
特定言之,如美國5,998,925號專利所揭示的二色法,係使用結合一Y3
Al5
O1 2
:Ce(YAG-Ce3 +
)磷光粉之InGaN為主的半導體材料的藍色發光二極體。將YAG-Ce3 +
磷光粉塗布在InGaN LED上,由磷光質將LED所發射的一部分藍光轉換為黃光。從LED發射的另一部分藍光的則透射穿過磷光質。此系統同時發射藍光(由LED發射)與黃光(由磷光質發射)。該藍色和黃色發射頻帶混合後,呈現給觀察者的是一般CRI值在約70左右及色溫Tc在大約6000 K到大約8000 K範圍的白光。
然而,先前技術的照明系統含有微晶磷光粉,由於它們不透明,因此有許多應用不能使用,這是先前技術的問題之一。不透明是因為微晶磷光粉的散射所造成。
DE 10349 038揭示了一種光源,其包含至少一種用於提供主要輻射之發光二極體及至少一種含有磷光質之多晶冷光轉換器,用於將該主要輻射轉換成次要輻射。此種多晶冷光轉換器提供較低的光線散射與吸收。該磷光質可為摻雜鈰的釔鋁石榴石(YAG-Ce3 +
)。
然而,先前技術用來改善照明系統透明度的解決辦法有顏色呈現不夠充分的缺點。
因此本發明之一目的即提供一用於產生白光的照明系統,其具有適當的光線萃取效能與透明度,且能夠呈現真實色彩。
本發明之另一目的係提供一用於產生紅色至琥珀色光的照明系統。
因此,本發提供一種包含一輻射源及一單塊陶瓷冷光轉換器之照明系統,該單塊陶瓷冷光轉換器含有至少一磷光質,其能夠吸收由該輻射源所發射的一部分光線,以及發射波長與該被吸收光線不同的光線;其中,該至少一磷光質為通式EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
的銪(II)-活化氧代氮化鋁矽酸鹽,其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬。
最好,該輻射源為一發光二極體。
依據本發明之一具體實施例,該單塊陶瓷冷光轉換器為一第一冷光轉換器元件,其進一步包含一或多個第二冷光轉換器元件。
該第二冷光轉換器元件可為一含有一第二磷光質的塗層。或者,該第二冷光轉換器元件可為一含有一第二磷光質的第二單塊陶瓷冷光轉換器。
本發明之另一方面提供一單塊陶瓷冷光轉換器,其含有至少一磷光質,能夠吸收由該輻射源所發射的一部分光線,以及發射波長與該被吸收光線不同的光線;其中,該至少一磷光質為通式EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
的銪(II)-活化氧代氮化鋁矽酸鹽,其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬。
該轉換器為一有效的轉換器,故其為能轉換高能輻射(例如電磁光譜中從UV到藍色範圍的輻射)的良好轉換器。該轉換器亦為有效得發射器,因其為光能量之良好發射器,該光能量係源自高能輻射輸入的轉換。若非如此,光線將被材料吸收,而影響整體轉換效率。
本發明係針對在任一包含主要輻射源之照明系統構造中,一種含有銪(II)-活化氧代氮化鋁矽酸鹽磷光質的單塊陶瓷冷光轉換器,該主要輻射源包括(但不限於)放電燈、螢光燈、無機和有機發光二極體、雷射二極體及X-射線管。本文中,術語「輻射」涵蓋電磁光譜中UV、IR和可見範圍的輻射。
目前雖然單塊陶瓷冷光轉換器預期可應用於廣泛種類的照明,但本發明係特別參考包含發光二極體的照明系統特定應用上作說明,特別是包含UV和藍色發光二極體的系統。
一般而言,單塊陶瓷冷光轉換器為一陶瓷體,它在受到高能電磁光子激發時,會發射可見或接近可見光譜的電磁輻射。
單塊陶瓷冷光轉換器的特徵為其典型的微結構。單塊陶瓷冷光轉換器之微結構為多晶,亦即,為一隱晶或奈米晶之不規則微晶集塊。微晶成長至緊密接觸而共用晶粒邊界。巨觀上,單塊陶瓷看似具有等向性,雖然利用SEM(掃描電子顯微鏡)很容易就可以偵測到多晶的微結構。
由於具有多晶的微結構,陶瓷冷光轉換器是透明的或至少具有很高的光學穿透性,其光吸收性很低。
包含通式為EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
(其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組之鹼土金屬)之銪(II)-活化氧代氮化鋁矽酸鹽磷光質的單塊陶瓷冷光轉換器具有高度的物理結實性,呈現加工性和磨光性等有用的材料性質,能夠改善光線萃取且有助於光導效應。
用於本發明的磷光質材料,其種類主要為氧-及鋁-取代之氮化矽酸鹽的銪(II)活化冷光材料。該磷光質的通式為EA2 - z
Si5 - a
Ala
N8 - a
Oa
:Euz
,其中0<a2,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬,其包含一主晶格,其中該主成分為矽和氮。該主晶格亦包含氧和鋁。一般認為該主晶格具有由(N-Si-N-)和(O-Si/Al-N)單元所組成的三維網絡結構,其中矽被氮和氧所四面包圍。
可製造出通式為EA2 - z
Si5 - a
Ala
N8 - a
Oa
:Euz
的一系列組成物,這些組成物形成範圍在0<a2和0<z0.2的完整的固熔體,其結晶屬斜方晶系。
表1將化學式為(Sr1 - x - y
Bax
)2
Si5 - a
Ala
N8 - a
Oa
:Euy
的組成物的結晶學資料、CIE 1931色座標和放射波長與先前技術的組成物(斜體字)作比較。
將氧和鋁結合到主晶格中會增加共價鍵結和配位場***的比例。結果導致激發與放射頻帶偏移至波長比基本氮化矽酸鹽晶格還長的範圍。
在三維網格中併入例如鹼土金屬及銪(II)等金屬離子以及最終之共活化劑。該等鹼土金屬較好是選自鈣、鍶及鋇。這些材料的主晶格可為六元素(2個陽離子)的氧代氮化鋁矽酸鹽,例如銪(II)-活化之鍶氧代氮化鋁矽酸鹽Sr2
Si3
Al2
N6
O2
:Eu,或可含有超過六種元素,例如銪(II)-活化之鍶-鋇氧代氮化鋁矽酸鹽(Sr,Ba)2
Si3
Al2
N6
O2
:Eu。
銪(II)的z比例較好是在0.05<z<0.2的範圍。當Eu(II)的z比例較低時,由於光致發光之激發放射中心的數目隨著銪(II)陽離子減少,因此光度會降低,而當z大於0.2時,會發生密度淬火。密度淬火指的是,為了提高螢光材料光度而添加的催化劑其濃度增加至超出最佳位準時,所發生的發射強度降低的現象。
該等銪(II)-活化之氧代氮化鋁矽酸鹽磷光質對電磁光譜能量部分的反應多於對光譜可見光部分的反應。
特定言之,依據本發明之磷光質尤其容易被波長200到420 nm的UV放射線所激發,但以具有400至495 nm波長的藍色發光組件所發射的LED光激發,其效率更高。因此該單塊陶瓷冷光轉換器的螢光材料具有能夠將氮化物半導體發光組件的藍光轉換成白光或黃色、琥珀色或紅色等彩色光的理想特性。
製造該單塊陶瓷冷光轉換器之第一步驟為準備一螢光微晶磷光粉材料,第二步驟為將該微晶材料施以均壓使其成為丸狀,並以高溫燒結該等丸狀材料一段足以緊縮成為一半透光體的時間。
該微結晶磷光粉的製造方法並無特別限制,可使用任何能夠提供本發明之磷光粉的方法來製造。
一種製造本發明的磷光質的較佳方法為固態法。此方法中,將磷光質前驅物在固態下混合並予以加熱,使該前驅物反應而形成磷光質材料粉末。
在一特定具體實施例中,該等紅色至黃-紅色發光磷光質係利用以下技術製成磷光粉:將高純度的鹼土金屬和銪(III)的硝酸鹽、碳酸鹽、草酸鹽和醋酸鹽溶解於25-30 ml的去離子水中並加以攪拌,製成混合的二價金屬氧化物。把溶液放在熱盤上加熱及攪拌,直到水蒸發掉而變成糊漿狀,視組成物而定,可能為白色或黃色糊漿。
以120℃烘乾該固體隔夜(12小時)。將所得固體物研磨成細粉後,置於高純度的氧化鋁坩堝中。把坩堝放到含木炭的盤子上,然後送進管爐以流動的氮氣/氫氣淨化數小時。爐子的參數為,以10℃/min升溫至1600℃,然後在1300℃維持4小時,之後把爐子關機,讓它冷卻到室溫。這些金屬氧化物與氮化矽Si3
N4
和氮化鋁AlN以預定的比例混合。將混合物放進高純度的氧化鋁坩堝中。把坩堝放到含木炭的盤子上,然後送進管爐以流動的氮氣/氫氣淨化數小時。爐子的參數為,以10℃/min升溫至1600℃,然後在1600℃維持4小時,之後把爐子關機,讓它慢慢冷卻到室溫。再次把樣品磨成細粉,然後以1600℃進行第二次退火。可以用稍低的溫度,於流動的氬氣中再進行額外的第三次退火,以改善光度輸出。
該磷光粉材料也可以用液態沉澱法製造。此方法中,把含有可溶磷光質前驅物的溶液經化學處理,使磷光質顆粒或磷光質顆粒前驅物沉澱。通常用高溫煅燒這些顆粒,製成磷光質化合物。
還有另外的方法是,把磷光粉顆粒前驅物或磷光質顆粒分散於泥漿中,然後噴灑該泥漿使液體蒸發而變乾燥。之後把形成的顆粒在固體狀態下以高溫燒結使粉末結晶而形成一磷光質。然後,以高溫燒結噴乾後的粉末,使其轉變成磷光質氧化物,使粉末結晶而形成磷光質。然後略為粉碎該等燒過的粉末,加以研磨,得到所需粒度的磷光質顆粒。
將這些方法製得的細粒微晶磷光粉用來製造本發明的陶瓷冷光轉換器。做法是對一適合的磷光粉施加非常高的壓力,加壓的同時以高溫熱處理,或加壓後再另外進行熱處理程序。最好是施以均壓。
尤佳的方法是熱均壓處理,或者冷均壓之後再進行燒結。亦可在冷均壓及燒結後再進行熱均壓。
緻密化程序必須仔細監督,以控制晶粒成長,以及除去殘留的孔隙。
該磷材料經過加壓及熱處理後,產生一單塊陶瓷體,該單塊陶瓷體很容易用現有的金屬相程序鋸開、加工和拋光。可以把該多晶陶瓷材料鋸成厚度1mm或更薄的晶圓。最好是將該陶瓷拋光而得到光滑的表面,以降低因表面粗糙所造成的繞射散射。
充分乾混以下重量的碳酸鍶和氧化銪:SrCO3
:20.0 g Eu2
O3
:0.487 g
將混合物置於氧化鋁坩堝中,於氮中含5%(體積)氫的還原空氣中以1200℃煅燒2小時。冷卻到室溫後,把得到的粉餅放到手套箱中,於乾燥的氮氣下搗碎成細粉。
把得到的氧化物粉末混合物,按下列重量與氮化矽於無水丙酮中進行溼混:(Sr,Eu)O:5.0 g Si3
N4
:3.77 g
把丙酮蒸發使該粉末混合物乾燥後,將它置於氧化鋁坩堝中,在氮中含5%(體積)氫的還原空氣中以1550℃燃燒2小時。把該磷光粉生料與一有機二醇結合劑混合,壓成丸狀,用44800 Psi(3.091×108
N/m2
)進行冷均壓以進一步壓密。然後將形成的原坏陶瓷體置於一鎢箔上,在與前述相同的還原空氣中以1700℃燃燒2小時。冷卻到室溫後,把得到的氮化陶瓷鋸成薄片。把這些薄片研磨拋光,得到最終的半透明氮化陶瓷。CLC微結構(圖2)呈現出統計上為粒狀結構的特徵,在1000:1的放大倍率下,顯現一粒狀邊界網格。該陶瓷展現Sr2
Si5
N8
的理論密度的97%密度(3.904 g/cm3
)。可藉由在氮氣中對該陶瓷施以熱均壓(溫度範圍1600-1780℃,壓力範圍2000到30000 PSI(138.00×105
到2.070×108
N/m2
)),以將剩餘孔隙去除,俾進一步提高樣品的密度。
該磷光陶瓷之特徵為粉末的X-射線繞射(Cu,Kα-線)。圖3顯示該單塊陶瓷冷光轉換器的X-射線繞射資料,與根據Sr2
Si5
N8
的結構資料所計算的XRD圖案進行比較。
圖3所示的X-射線繞線圖案與Sr2
Si5
N8
的已計算XRD圖案相符,位置與強度有一定量的小幅偏離,是因為銪取代鍶的緣故。
燒結後的磷光質以能夠產生365奈米尖峰波長之紫外光的水銀燈加以激發。使用Minolta機型CS-100-A的光度計來量測該磷光質的光致發光。
銪(II)-活化氧代氮化鋁矽酸鹽型式的各磷光質在被UVA或電磁光譜的藍色範圍激發時,會發射黃、琥珀至深紅色的螢光。
當以波長495 nm的輻射加以激發時,發現該等銪(II)-活化氧代氮化鋁矽酸鹽磷光質可提供一寬頻帶放射,其峰值波長為640 nm,尾部放射波長達到750 nm。
這些銪-活化氧代氮化鋁矽酸鹽磷光質可以用波長在370 nm和490 nm之間的輻射有效地加以激發。
本發明之一方面提供一包含一輻射源及一單塊陶瓷冷光轉換器的照明系統,該單塊陶瓷冷光轉換器含有至少一磷光質,其能夠吸收由該輻射源所發射光線之一部分,以及發射波長與該被吸收光線不同的光線;其中該至少一磷光質為通式EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
之銪(II)-活化氧代氮化鋁矽酸鹽,其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬。
輻射源較佳包括半導體光學輻射發射器及其他受電力激發時會發射光學輻射的裝置。半導體光學輻射發射器包括發光二極體LED晶片、發光聚合物(LEP)、雷射二極體(LD)、有機發光裝置(OLED)、聚合物發光裝置(PLED)等。
此外,用在放電燈與螢光燈中的發光組件,諸如水銀低壓和高壓放電燈、硫放電燈,以及以分子輻射體為主的放電燈等,預期亦可作為輻射源,與本發明之磷光組成物一起使用。
在本發明之較佳具體實施例中,該輻射源為一發光二極體。
任一包括一發光二極體或一發光二極體陣列之照明系統的組態,以及包含一銪(II)-活化氧代氮化鋁矽酸鹽磷光組成物的陶瓷冷光轉換器,都視為在本發明的範圍內,最好是加入其他眾所熟知的磷光質,該等磷光質組合之後,在受到如前述由LED所發射的主要UV或藍光照射時,可獲得一特定顏色的光或白光。
可用以將該單塊陶瓷冷光轉換器耦接至一發光二極體或一發光二極體陣列的可能組態包括以導線架黏著的LED以及以表面黏著的LED。
以下說明圖1所示之包含一輻射源及一單塊陶瓷冷光轉換器之此照明系統之一具體實施例的詳細構造。
圖1顯示一覆晶型發光二極體連同一陶瓷冷光轉換器的示意圖。
該發光二極體以表面黏著於一基板上。該單塊陶瓷冷光轉換器係做成板狀,其設置的方式係使從該二極體發射的大部分光線都能夠以大約垂直於該板表面的角度射入該板中。為達此目的,在該發光二極體周圍設置一反射器,以便把從該二極體發射的光線朝離開板的方向反射。
操作時,施加電力於晶粒以啟動該晶粒。晶粒啟動時會發射主要光線,例如藍光。該已發射主要光線的一部分完全或部分被該陶瓷冷光轉換器所吸收。該陶瓷冷光轉換器接著回應該主要光線之吸收而發射次要光線,亦即,轉換後的光線具有較長的峰值波長,主要是頻帶夠寬的黃光(明確言之,紅光佔很大的比例)。該已發射主要光線的其餘未被吸收部分與該次要光線一起透射穿過該陶瓷冷光轉換器。
該反射器將一般方向上未被吸收之該主要光線及該次要光線引導成為一輸出光線。因此,該輸出光線為從晶粒發射的主要光線及從螢光層發射的次要光線所組成的複合光線。
依據本發明之照明系統,其所輸出光線的色溫或色點會視該次要光線相較於該主要光線的光譜分布與強度而改變。
首先,藉由適當地選擇發光二極體,可以改變該主要光線的色溫或色點。
其次,藉由適當地選擇該陶瓷冷光轉換器中的磷光組成物,可改變該次要光線的色溫或色點。
此外,這些配置有利地提供使用一第二冷光轉換器的可能性,因此有助於甚至更精確地設定所需色調。
依據本發明之一方面,該照明系統之輸出光線具有一可顯現為「白」光的光譜分布。
在依據本發明之一發白光的照明系統之第一具體實施例中,藉由選擇發光材料,使得由一藍色發光二極體所發射之一藍色輻射轉換為互補的波長範圍,以形成二色白光,可有利地產生該裝置。
此例中,黃光係利用單塊陶瓷冷光轉換器的磷光材料所產生,其包含通式為EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
之一磷光質,其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬。
此外,亦可使用一第二紅色螢光材料,以進一步改善此照明系統的色彩呈現。
採用最大發射波長在380至480 nm的藍色LED可達到尤佳結果。對於特定採用銪(II)-活化氧代氮化鋁矽酸鹽的激發光譜而言,已發現最佳結果為445至468 nm。
藉由將依據本發明之一尺寸為4x4x0.3mm的經拋光陶瓷冷光轉換器裝在一發射458 nm波長之W(Al,In,Ga)N LED晶片上,可特佳實現本發明之發白光的照明系統。
由一458 nm波長(Al,In,Ga)N發光二極體所發射的一部分藍色輻射被該銪(II)-活化氧代氮化矽酸鋁鹽偏移至橘色到紅色光譜範圍中,因而進入一波長範圍相對於藍色而言是互補的範圍。個人觀察者將藍色主要光線與發射橘光的磷光質所發射的次要光線的組合感知為白光。
當與包含YAG:Ce作為一陶瓷冷光轉換器之先前技術的照明系統所產生的白光輸出的光譜分布作比較時,光譜分布的明顯差異是峰值波長的偏移,該峰值波長係在可見光譜的紅光範圍中。因此,與先前技術所產生的光輸出比較,由該照明系統所產生的白光輸出具有明顯額外大量的紅色光。
在一第二具體實施例中,藉由選擇發光材料,使得由一藍色發光二極體所發射之一藍色輻射轉換為互補的波長範圍,以形成多色白光,可有利地產生本發明之發白光的照明系統。此例中,橘色到紅色光係利用螢光材料產生,其包含磷光質混合物,包括作為一第一單塊陶瓷冷光轉換器的銪(II)-活化氧代硝化鋁矽酸鹽磷光質與在一第二冷光轉換器中之一第二磷光質。
該第二冷光轉換器可以用一第二單塊陶瓷冷光轉換器的形式提供,或以一傳統的磷光塗層的形式提供。
以下表2摘要列出常用的第二磷光質及其光學特性。
本發明之又一方面提供一種照明系統,其所發射的輸出光顯現「黃至紅」光的光譜分布。
包含通式為EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
之銪(II)-活化氧代氮化鋁矽酸鹽(其中0<a4,0<b4,0<z0.2;EA為至少一選自鈣、鋇及鍶所組成群組的鹼土金屬)之單塊陶瓷冷光轉換器作為磷光質,特別適合由例如發射UVA的LED或發射藍光的LED等之一主要UVA或藍色輻射源激發,而作為黃色成分。
因此有可能實施發光範圍係在電磁光譜中黃到紅光的照明系統。
藉由選擇發光材料,使得由藍色發光二極體所發射之一藍色輻射轉換為互補的波長範圍,以形成二色黃光,可有利地產生本發明之發黃光的照明系統。
此例中,黃光係利用包含一鐿-活化氧代氮化鋁矽酸鹽磷光質的發光材料而產生。
採用最大發射波長在400至480 nm的藍色LED可達到尤佳結果。對於鹵素氧代氮化鋁矽酸鹽的激發光譜而言,已發現445至465 nm可得最佳結果。
圖4顯示一包含通式為EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
之銪(II)-活化氧代氮化鋁矽酸鹽(其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬)的單塊陶瓷冷光轉換器的發射光譜。
圖5顯示一包含通式為EA2 - z
Si5 - a
Ala
N8 - b
Ob
:Euz
之銪(II)-活化氧代氮化鋁矽酸鹽(其中0<a4,0<b4,0<z0.2;EA為至少一種選自鈣、鋇及鍶所組成群組的鹼土金屬)的單塊陶瓷冷光轉換器,結合一藍色發光二極體在50到300 mA的不同驅動電流下的發射光譜。系統的色點與正向電流無關。相關的色點為x=0.675、y=0.317。
LED-磷光系統的色彩輸出對磷光層之厚度很敏感,若磷光層較厚並且包含過多的黃色鐿活化氧代氮化鋁矽酸鹽磷光質,則穿過該厚磷光層的藍色LED的光量會較少。於是經組合LED-磷光系統將顯現黃至紅色光,因為結果是由該磷光質之黃至紅色的次要光線所支配。因此,該磷光層的厚度是影響系統之顏色輸出的一個關鍵變數。
此情況中,藉由根據混合物與濃度來適當地選擇磷光質,可以改變所產生的黃光的色調(CIE色度圖中的色點)。
在另一具體實施例中,藉由選擇輻射源,以使得由放射UV的二極體所發射的UV輻射完全由依據本發明之一單塊陶瓷冷光轉換器轉換成黃至紅的單色光,可有利地產生本發明之發射黃至紅色光的照明系統。
圖1為包含本發明之陶瓷冷光轉換器的二色白色LED燈的側面示意圖,該LED燈係設置於由發光二極體覆晶結構所發射光線的路徑中。
圖2顯示蝕刻陶瓷冷光轉換器的微結構,放大倍率為1000:1。
圖3顯示以Cu Kα輻射量測本發明之陶瓷冷光轉換器所得之XRD圖案,以及計算得到的Sr2
Si5
N8
的XRD圖案。
圖4顯示本發明之陶瓷冷光轉換器的發射光譜(λexc
=450nm)。
圖5顯示638nm的紅色CLC照明系統a)在50到300mA的不同驅動電流下的發射光譜及b)其輸出特徵。
Claims (9)
- 一種包含一輻射源及一單塊陶瓷冷光轉換器之照明系統,該單塊陶瓷冷光轉換器包含至少一磷光質,其能夠吸收由該輻射源所發射之一部分光線及發射波長不同於該被吸收光線的光線;其中該至少一磷光質為通式EA2-z Si5-a Ala N8-b Ob :Euz 之銪(II)-活化氧代氮化鋁矽酸鹽,其中0<a4,0<b4,0<z0.2;EA為至少一種選自由鈣、鋇及鍶所組成群組之鹼土金屬。
- 如請求項1之照明系統,其中該輻射源係發光二極體。
- 如請求項1之照明系統,其中該單塊陶瓷冷光轉換器為一第一冷光轉換器元件,其進一步包含一或多個第二冷光轉換器元件。
- 如請求項3之照明系統,其中該第二冷光轉換器元件為含有磷光質之塗層。
- 如請求項3之照明系統,其中該第二冷光轉換器元件為含有第二磷光質之第二單塊陶瓷冷光轉換器。
- 一種包含至少一磷光質之單塊陶瓷冷光轉換器,該磷光質能夠吸收由輻射源所發射之一部分光線及發射波長不同於該被吸收光線的光線;其中該至少一磷光質為通式EA2-z Si5-a Ala N8-b Ob :Euz 之銪(II)-活化氧代氮化鋁矽酸鹽,其中0<a4,0<b4,0<z0.2;EA為至少一種選自由鈣、鋇及鍶所組成群組之鹼土金屬。
- 一種製備如請求項6之單塊陶瓷冷光轉換器之方法,該方法包括:第一步驟為準備一螢光微晶磷光粉材料,第 二步驟為將該微晶材料施以均壓使其成為丸狀,並以高溫燒結該等丸狀材料一段足以緊縮成為一半透光體的時間。
- 如請求項7之方法,其中進行一或多個(i)熱均壓處理或(ii)冷均壓處理之後再進行燒結。
- 如請求項7或8之方法,其中先在冷均壓及燒結後再進行熱均壓。
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EP (1) | EP1838808B1 (zh) |
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JP2008527706A (ja) | 2008-07-24 |
ATE513026T1 (de) | 2011-07-15 |
TW200703403A (en) | 2007-01-16 |
EP1838808A1 (en) | 2007-10-03 |
CN101103088A (zh) | 2008-01-09 |
WO2006072918A1 (en) | 2006-07-13 |
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