TWI535826B - 磷光體組成物、發光裝置以及產生光的方法 - Google Patents
磷光體組成物、發光裝置以及產生光的方法 Download PDFInfo
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- TWI535826B TWI535826B TW100123873A TW100123873A TWI535826B TW I535826 B TWI535826 B TW I535826B TW 100123873 A TW100123873 A TW 100123873A TW 100123873 A TW100123873 A TW 100123873A TW I535826 B TWI535826 B TW I535826B
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Description
本申請案主張2010年7月9號提申的美國專利申請案第61/363,148號的優先權。該申請案的整體內容在此併入本案以供參考。
本發明是有關於一種同時摻雜鈰(Ce)和錳(Mn)的石榴石氧化物磷光體組成物及其製造方法。本發明也關於一種包括上述組成物的發光元件。
固態發光元件,如發光二極體(LED)、有機發光二極體(OLED,有時或稱有機電致發光元件,OEL)及無機電致發光元件(IEL)已廣泛用於各種用途,如平板顯示器、各種儀器的指示器、招牌及裝飾燈飾等。改進這些發光元件(尤其LED)的效率可提供更高的、與一般用途的發光元件(如螢光燈及白熾燈)相匹配的發光強度。白光LED,特別是具有高演色性指數(color rendering index;CRI)及低相關色溫(correlated color temperature;CCT)的白光LED,有希望可取代現存一般用途的發光元件。
傳統白光LED包括藍光LED與發黃光的釔鋁石榴石(YAG)磷光體粉末(分散在封裝樹脂中)的組合,封裝樹脂包括環氧樹脂或矽氧樹脂(例如美國專利第5,998,925號及第6,069,440號)。然因缺乏紅光,這種YAG:Ce型LED系統具有低CRI。因此,需要能提供寬發射光譜(橫
跨寬的波長範圍)的磷光體和用以製備磷光體的簡單製程。
將鈰作為活化劑以提供寬放射光譜(峰值位置從綠光(約480nm到約580nm)到橘光區(約585nm到約625nm))是獲得寬放射光譜的一種方法。因Ce離子的放光與電子在5d軌域中的躍遷有關,放射光譜可因主體晶格中的其他陽離子而偏移。美國專利7,029,602號記載,受藍光LED激發時,Lu2CaAl4SiO12:Ce發出綠光。因此,相較於Y3Al5O12:Ce,Lu2CaAl4SiO12:Ce的發光顯現了藍位移,這是因為Lu離子的尺寸較小的緣故。
依晶體結構和晶格位置,錳離子的放光常在綠或紅光區。理論上錳離子可因此改善現存磷光體的放射光譜。然錳離子對藍光吸收很差,僅在受紫外光激發時放光,故一般不用於以藍光LED激發發光磷光體的習知白光LED。
本文的一些實施例包括一種磷光體組成物,其包括化學式(RE2-x+yCexAk1-y)(MG4-zSirMnz)(Si1-ePe)O12-rNr表示的化合物。其中RE包括至少一稀土金屬。Ak包括至少一鹼土金屬。MG包括至少一主族元素。x大於0且小於等於0.2。y<1。z大於0且小於等於0.8。e約等於0,或小於等於0.16。r約等於0,或小於等於1。而z約等於e+y。
在一些實施例中,MG是選自由鋁、鈧、銦、鎵、硼、矽及其組合所組成的族群。在一些實施例中,MG為鋁。
在一些實施例中,RE是選自由鎦(Lu)、釔(Y)、釓(Gd)、鋱(Tb)、釤(Sm)、鐠(Pr)及其組合所組成的族群。在
一些實施例中,RE為鎦。
在一些實施例中,Ak選自由鎂、鈣、鋇、鍶及其組合所組成的族群。在一些實施例中,Ak為鈣。
一些實施例中,r0。一些實施例中,e0。
在一些實施例中,上述化合物是以化學式(Lu2.16-xCex)Ca0.84Al3.84Mn0.16SiO12表示,其中x大於0.0025且小於0.2。在一些實施例中,x約等於0.16。
一些實施例中,上述化合物以化學式(Lu1.84+zCe0.16)Ca1-z(Al4-zMnz)SiO12表示,其中z大於0且小於0.8。一些實施例中,z約等於0.04。一些實施例中,z約等於0.02。
在一些實施例中,e大於0。在一些實施例中,上述化合物是以化學式(Lu1.84Ce0.16)Ca(Al4-zMnz)(Si1-zPz)O12表示,其中z至少約等於0.01且小於約0.16。在一些實施例中,z約等於0.02。在一些實施例中,z約等於0.04。
一些實施例中,r>0.001。一些實施例中,e0。一些實施例中,x0.16。一些實施例中,r0.4。在一些實施例中,r1。在一些實施例中,z0.16。
一些實施例中,上述化合物以選自由(Lu1.86Ce0.16Ca0.98)(Al3.98Mn0.02)SiO12、(Lu1.88Ce0.16Ca0.96)(Al3.96Mn0.04)SiO12、(Lu1.84Ce0.16)Ca(Al3.98Mn0.02)(Si0.98P0.02)O12及(Lu1.84Ce0.16)Ca(Al3.96Mn0.04)(Si0.96P0.04)O12組成的族群的化學式來表示。
一些實施例中,上述化合物以化學式(Lu2-x+zCexCa1-z)(Al4-z-rSirMnz)SiO12-rNr表示,其中x>約0.001且小於約0.4。z>約0.001且小於約0.4。r>約0.2且小於等於約1。
一些實施例中,上述化合物以選自由(Lu2.0Ce0.16Ca0.84)(Al3.44Si0.40Mn0.16)SiO11.6N0.40及(Lu2.0Ce0.16Ca0.84)(Al2.84Si1.0Mn0.16)SiO11N1所組成的族群的化學式來表示。
在一些實施例中,磷光體組成物包括:包括上述化合物的微粒。
在一些實施例中,磷光體組成物是燒結陶瓷板。
在一些實施例中,當上述化合物暴露於具有約450nm波長的輻射時,會放射峰值波長介於約500nm與約650nm之間的輻射。
在一些實施例中,上述化合物具有介於約515nm與約560nm之間的第一峰值發射波長,以及介於約600與約615nm之間的第二峰值發射波長。
本文揭露的一些實施例包括發光裝置,其包括:用以放射藍光輻射的光源,以及用以接收至少一部份藍光輻射的磷光體組成物。在一些實施例中,藍光輻射具有介於約430nm與約550nm之間的峰值發射波長。在一些實施例中,藍光輻射具有約為450nm的峰值發射波長。在一些實施例中,發光裝置具有至少為90的演色性指數(CRI)。
本文揭露的一些實施例包括一種產生光的方法,其包括將磷光體組成物暴露於藍光輻射下。在一些實施例中,藍光輻射的峰值發射波長介於約430nm與550nm之間。在一些實施例中,藍光輻射的峰值發射波長約為450nm。在一些實施例中,光具有至少為90的演色性指數。
本文揭露具有寬放射光譜且可被藍光激發的磷光體組成物。申請人意外發現,添加錳於鈰摻雜石榴石磷光體(特別是Lu2CaAl4SiO12)可使其在受到藍光激發時提供寬放射光譜。特別是,上述寬放射光譜可具有兩個峰值放射波長,其可能由共摻質鈰及錳所貢獻。雖不願被任何特定理論所限,但一般相信,鈰離子吸收藍光輻射後將能量轉移給錳離子,否則錳離子在藍光輻射下不會發光。因此,從標準藍光LED接受藍光輻射時,摻質鈰及錳的組合協同作用而提供寬放射光譜。反之,只摻錳離子的磷光體僅在紫外輻射下發光,而只摻鈰離子的磷光體的放射光譜較窄。
本案的磷光體組成物實施於標準LED發光元件時,可提供比現存磷光體優越的發光特性。例如,相較於現存磷光體,其可具有優良的CRI。因此,該磷光體組成物具有優越的性質,可提供適於一般發光用途的優良發光元件。
在一些實施例中,該磷光體組成物可以用化學式I:(RE2-x+yCexAk1-y)(MG4-z-rSirMnz)(Si1-ePe)O12-rNr表示,其中RE包括至少一稀土金屬。Ak包括至少一鹼土金屬。MG包括至少一主族元素。x大於0且小於等於0.2。y小於1。z大於0且小於等於0.8。e等於0或小於等於0.16。r等於0或小於等於1。而z約為e與y的和。
一些實施例中,MG選自鋁、鈧、銦、鎵、硼、矽及其組合。在一些實施例中,MG為鋁。一些實施例中,MG
為鈧、銦、鎵、硼或矽。MG亦可是選自鋁、鈧、銦、鎵、硼及矽的至少兩種(如二、三、四、五或六種)元素的組合。例如,MG可為第一元素與第二元素的組合,第一與第二元素之任一均選自鋁、鈧、銦、鎵、硼及矽。第一第二元素的莫耳比例如可以是:至少約10:90、至少約20:80、至少約40:60或至少約1:1。第一第二元素的莫耳比例如還可以是:至多約90:10、至多約80:20、至多約60:40或至多約1:1。在一些實施例中,MG是第一元素為鋁的組合。在一些實施例中,MG是第二元素為銦的組合。在一些實施例中,MG是第二元素為鎵的組合。例如,MG可以是鋁及鎵(莫耳比約1:1)的組合。
一些實施例中,RE選自鎦、釔、釓、鋱、釤、鐠及其組合。一些實施例中,RE是鎦。RE亦可為選自鎦、釔、釓、鋱、釤及鐠的至少兩種(例如二、三、四、五或六種)元素的組合。例如,RE可為第一元素與第二元素的組合,第一與第二元素之任一均選自鎦、釔、釓、鋱、釤及鐠。第一第二元素的莫耳比例如可以是:至少約10:90、至少約20:80、至少約40:60或至少約1:1。第一第二元素的莫耳比例如還可以是:至多約90:10、至多約80:20、至多約60:40或至多約1:1。在一些實施例中,RE是第一元素為鎦的組合。在一些實施例中,RE是第二元素為釔的組合。例如,RE可以是鎦及釔(莫耳比約1:1)的組合。
一些實施例中,Ak是選自鎂、鈣、鋇、鍶及其組合。一些實施例中,Ak是鈣。一些實施例中,Ak是鎂。Ak亦
可為選自鈣、鋇及鍶的至少兩種(如二或三種)元素的組合。例如,Ak可以是第一元素與第二元素的組合,第一與第二元素之任一均選自鈣、鋇及鍶。第一第二元素的莫耳比例如可以是:至少約10:90、至少約20:80、至少約40:60或至少約1:1。第一第二元素的莫耳比例如還可以是:至多約90:10、至多約80:20、至多約60:40或至多約1:1。一些實施例中,Ak是第一元素為鈣的組合。一些實施例中,Ak是第二元素為鋇的組合。例如,Ak可以是鈣及鋇(莫耳比約1:1)的組合。
在一較佳實施例中,MG是鋁、RE是鎦且Ak是鈣。例如,一些較佳的磷光體組成物可由化學式II:(Lu2-x+yCexCa1-y)(Al4-z-rSirMnz)(Si1-ePe)O12-rNr來表示,其中x大於0且小於等於0.2。y小於1。z大於0且小於等於0.8。e等於0或小於等於0.16。r等於0或小於等於1。而z約為e與y之合。
化學式I及II所表成分的相對量並無特別限制。依本案之教示,具通常知識者可依據其想要的發光用途,為磷光體組成物的每一成份選擇適當的量。例如,如實例2所示,可改變共摻質的相對量以調整放射光譜中峰的相對大小和量子效率。同理,如另一實例,主體晶格的組成也會改變放射光譜的相對峰值。
因此,增加Ce3+的量導致Ce3+放射波長的紅位移。而增加Mn2+的量導致Ce3+放射波長的藍位移與Mn2+放射波長的紅位移。在主體改質的情況中,添加釓或鋱增加了
Mn2+的放射。
然而,在一些實施例中,添加錳摻質於化學式I的磷光體組成物中會產生電荷不平衡,其較佳是藉由調整RE、Ak和P相對於鈰和錳的量來中和之。
變數x例如可以是:至少約0.001、至少約0.01或至少約0.02。變數x例如也可以是:至多約0.18或至多約0.16。x的例示值包括(但不限於)約0.08及約0.16。
在一些實施例中,變數y約等於z與e的差(例如y=z-e)。變數y例如可以是:至少約0.001、至少約0.01或至少約0.02。變數y例如也可以是:至多約0.8、至多約0.4及至多約0.2。y的例示值包括(但不限於)0、約0.02、約0.04及約0.16。在一些實施例中,y約等於z。
變數z例如可以是:至少約0.001、至少約0.01或至少約0.02。變數z例如也可以是:至多約0.5或至多約0.4。z的例示值包括(但不限於)約0.02、約0.04及約0.16。在一些實施例中,z約為e與y之合。在一些實施例中,z約等於e。在一些實施例中,z約等於y。
在一些實施例中,變數e等於z與y的差(例如e=z-y)。變數e例如可以是:至少約0.001、至少約0.01或至少約0.02。變數e例如也可以是:至多約0.16、至多約0.12或至多約0.08。e的例示值包括(但不限於)0、約0.02及約0.04。在一些實施例中,e約等於z。
變數r例如可以是:至少約0.001、至少約0.01、至少約0.1或至少約0.2。變數r例如也可以是:至多約1或
至多約0.6。r的例示值包括(但不限於)0、約0.4及約1。
在一些實施例中r等於0。例如,磷光體組成物可由化學式III:(RE2-x+yCexAk1-y)(MG4-zMnz)(Si1-ePe)O12表示,其中RE、Ak、MG、x、y、z及e可與化學式I定義者相同。以化學式III表示的磷光體組成物的非限制性實例包括(Lu1.86Ce0.16Ca0.98)(Al3.98Mn0.02)SiO12、(Lu1.88Ce0.16Ca0.96)(Al3.96Mn0.04)SiO12、(Lu1.84Ce0.16)Ca(Al3.98Mn0.02)(Si0.98P0.02)O12及(Lu1.84Ce0.16)Ca(Al3.96Mn0.04)(Si0.96P0.04)O12。
一些實施例中,e等於0。例如,磷光體組成物可由化學式IV:(RE2-x+zCexAk1-z)(MG4-z-rSirMnz)SiO12-rNr表示,其中RE、Ak、MG、x、y、z及r可與化學式I的任一實施例相同。此種磷光體組成物的實例包括(但不限於):(Lu1.86Ce0.16Ca0.98)(Al3.98Mn0.02)SiO12、(Lu1.88Ce0.16Ca0.96)(Al3.96Mn0.04)SiO12、(Lu2.0Ce0.16Ca0.84)(Al3.44Si0.40Mn0.16)SiO11.6N0.40及(Lu2.0Ce0.16Ca0.84)(Al2.84Si1.0Mn0.16)SiO11N1。
在一些實施例中,r=0且e=0。磷光體組成物例如可由化學式V:(RE2-x+zCexAk1-z)(MG4-zMnz)SiO12表示,其中RE、Ak、MG、x及z與化學式I定義者相同。一些實施例中,磷光體組成物可由化學式V表示,其中z約為0.16,而x大於約0.025且小於約0.2,或者x較佳等於約0.16。一些實施例中,x約0.16,而z大於0且小於約0.8。一些實施例中,z約為0.02或z約為0.04。化學式V表示的例示性磷光體組成物包括(但不限於):(Lu1.86Ce0.16Ca0.98)(Al3.98Mn0.02)SiO12及(Lu1.88Ce0.16Ca0.96)(Al3.96Mn0.04)SiO12。
在一些實施例中,e大於0且r=0。例如,磷光體組成物可由化學式VI:(RE2-x+yCexAk1-y)(MG4-zMnz)(Si1-ePe)O12的化合物表示,其中RE、Ak、MG、x、y、z及e與化學式I定義者相同。一些實施例中,磷光體組成物由化學式VI表示且y約等於0。例如,磷光體組成物由化學式VII:(RE2-xCexAk)(MG4-zMnz)(Si1-zPz)O12表示,其中RE、Ak、MG、x及z與化學式I定義者相同。在一些實施例中,x可為約0.08或約0.16。一些實施例中,z大於約0.01且小於約0.16、約0.02或約0.04。以化學式VI和VII表示的例示磷光體組成物包括(但不限於):(Lu1.92Ce0.08)Ca(Al3.98Mn0.02)(Si0.98P0.02)O12、(Lu1.92Ce0.08)Ca(Al3.96Mn0.04)(Si0.96P0.04)O12、(Lu1.84Ce0.16)Ca(Al3.98Mn0.02)(Si0.98P0.02)O12及(Lu1.84Ce0.16)Ca(Al3.96Mn0.04)(Si0.96P0.04)O12。
一些實施例中,r大於約0.001。一些實施例中,r大於約0.001且e=0。例如,磷光體組成物可由化學式VIII:(RE2-x+zCexAk1-z)(MG4-z-rSirMnz)SiO12-rNr表示,其中RE、Ak、MG、x、z及r可與化學式I的任一實施例相同。一些實施例中,磷光體組成物由化學式VIII表示,其中r約為0.4。一些實施例中,磷光體組成物由化學式VIII表示,其中r約為0。一些實施例中,磷光體組成物由化學式VIII表示,其中x約0.16。一些實施例中,磷光體組成物由化學式VIII表示,其中z大於約0.001且小於約0.4(z較佳約為0.16)。以化學式VIII表示的磷光體組成物的非限制性實例包括:(Lu2.0Ce0.16Ca0.84)(Al3.44Si0.40Mn0.16)SiO11.6N0.40
及(Lu2.0Ce0.16Ca0.84)(Al2.84Si1.0Mn0.16)SiO11N1。
本案的磷光體組成物的優勢在於,當受到藍光輻射的激發時可具有寬放射光譜。在一些實施例中,當暴露於具有約450nm的波長的輻射時,磷光體組成物可放射峰值波長介於約500nm與約650nm之間的輻射。在一些實施例中,磷光體組成物可具有介於約515nm與約560nm之間的第一峰值放射波長,以及介於約600nm與約615nm之間的第二峰值放射波長。在一些實施例中,組成物具有介於約730nm與約770nm之間的第三峰值放射波長。
磷光體組成物還可具有高的演色性指數(CRI)及/或低的相關色溫(correlated color temperature;CCT)。當暴露於藍光輻射時,磷光體組成物可具有至少約70的CRI。藍光輻射例如可具有在350nm至550nm的範圍間,或約450nm的峰值波長。在一些實施例中,CRI為至少約80、至少約85、至少約90或約91。同時,參考CCT可在2500K至約10000K、約2500K至約5000K、約2500K至約4500K或約2600K至約3400K的範圍中。
在一些實施例中,磷光體組成物可呈微粒形態(例如粉末)。微粒例如可具有小於約1mm、小於約500μm、小於約100μm或小於約1μm的平均粒徑。微粒例如還可具有至少1nm、至少50nm、至少100nm、至少500nm或至少1μm的的平均粒徑。在一些實施例中,微粒具有在約1nm至約1mm的範圍中的平均粒徑。如以下關於發光裝置的進一步討論,磷光體粉末可被封裝(或分散)在樹
脂(如環氧樹脂)中。
磷光體組成物可包括不同量的一或多種以化學式I到VIII中任一者所表示的化合物。在一些實施例中,磷光體組成物包括至少約1wt%的一或多種以化學式I到VIII中任一者所表示的化合物。在一些實施例中,磷光體組成物包括至少約10wt%的一或多種以化學式I到VIII中任一者所表示的化合物。在一些實施例中,磷光體組成物包括至少約25wt%的一或多種以化學式I到VIII中任一者所表示的化合物。在一些實施例中,磷光體組成物包括至少約50wt%的一或多種以化學式I到VIII中任一者所表示的化合物。在一些實施例中,磷光體組成物包括至少約75wt%的一或多種以化學式I到VIII中任一者所表示的化合物。
在一些實施例中,每一磷光體組成物在放射峰值波長附近的總光穿透率,或在光致發光光譜的峰值波長附近的總光穿透率,可至少約為總光穿透率之理論值的25%、至少約為該理論值的40%或至少約為該理論值的60%。
本申請案的磷光體組成物(如以化學式I到VIII中任一者所示者)可以熟悉本技術領域者習知的方法來製備。例如,磷光體組成物可使用習知用來製造磷光體的固態反應製程,結合例如元素氧化物、碳酸、及/或氫氧化物作為起始材料來製造。其他起始材料可包括硝酸鹽(nitrates)、硫酸鹽(sulfates)、醋酸鹽(acetates)、檸檬酸鹽(citrates)或草酸鹽(oxalates)。另外,稀土氧化物的共沉澱物可用
來當作RE元素的起始材料。Si可藉由SiO2、矽酸或其他來源材料(如燻矽(fumed silica))來提供。
製造上述磷光體的一實例製程使用陣列漿液法(array slurry method)。將原料(例如Lu2O3、Y2O3、Gd2O3、Tb4O7、Sm2O3、Pr6O11、CaCO3、BaCO3、SrCO3、MnCO3、Si3N4、CeO2、MgO、SiO2及Al2O3)研磨成微米粉末,再以最多16wt%的固體添加量將其分散在水中。可以商用的液體處理器將漿液在劇烈攪拌下噴灑至氧化鋁坩鍋中。於水分蒸發後,在還原環境(例如,空氣中約1%氫氣)下以約1200℃到約1700℃加熱漿液,而產生均質的固態混合物。
另一實例製程是以乾或溼混合製程結合起始材料,並在空氣中(或還原環境下)以約1000℃到約1600℃烘烤。在混合步驟前或其中,可添加助熔劑(fluxing agent,例如燒結助劑)於混合物中。在一些實施例中,燒結助劑可包括(但不限於)矽酸四乙酯(TEOS)、矽酸膠、氧化鋰、氧化鈦、氧化鋯、氧化鎂、氧化鋇、氧化鈣、氧化鍶、氧化硼或氟化鈣。其他燒結助劑包括(但不限於)金屬鹵化物(如NaCl、KCl、AlF3或NH4Cl)及有機化合物(如尿素)。一些實施例中,磷光體組成物包括助熔劑物質(flux material)或燒結助劑,其重量比例介於約0.01%與約5%之間、介於約0.05%與約5%之間、介於約0.1%與約4%之間或介於約0.3%與約1%之間。燒結助劑可與原料混合。例如,在一些實施例中,可加入矽酸四乙脂於原料中以提供所欲的燒結助劑量。在一些實施例中,提供重量比例約
0.05%到約5%的TEOS給磷光體組成物。在一些實施例中,TEOS的量可以在約0.3%到約1%的重量比例之間。
起始材料可用任何機械方法混合,包括(但不限於):在高速混合器或帶式混合器(Ribbon Blender)中攪拌或混合。起始材料可在球磨機、鎚磨機或噴射磨機中結合並被粉碎。混合可以濕磨進行,其時點較佳是在將起始材料的混合物製成用於後續沈澱的溶液時。如果混合物是溼的,可先將其乾燥,再在還原環境下以約900℃到約1700℃(較佳是從約1000℃到約1600℃)加熱一段足以使所有混合物實質上轉變成最終組成物的時間。
加熱可在批次或連續製程中進行,較佳配合攪拌或混合動作以促成良好的氣固(gas-solid)接觸。加熱時間取決於要被加熱的混合物的量、氣體在加熱儀器中傳輸的速率及加熱儀器中氣固接觸的品質。一般來說,約10小時的加熱時間是適當的。還原環境一般包括還原氣體,如氫氣、一氧化碳或其組合,可選擇以惰性氣體(如氮氣、氦氣或其組合)稀釋。另外,可將容納混合物的坩鍋包裝在含高純度碳顆粒的第二密封坩鍋中,且在空氣中加熱,使碳顆粒與空氣中的氧氣反應而產生提供還原環境的一氧化碳。
在一些實施例中,可在硝酸溶液中攪拌與分解起始材料。酸液的強度以熟悉本技術領域者的技術知識來選擇,以快速溶解含氧化合物。接著,在酸液中逐量加入氨水。氨水也可以由有機鹼取代,例如甲醇胺、乙醇胺、丙醇胺、二甲醇胺、二乙醇胺、二丙醇胺、三甲醇胺、三乙醇胺、
三丙醇胺。
接著,酸液中的沉澱物可經過濾、去離子水清洗及乾燥。乾燥的沉澱物可被粉碎(例如球磨或其他徹底混合),然後在空氣中以約400℃到約1600℃煆燒一段足以確保起始材料實質上完全脫水的時間。煆燒可在定溫下進行。或者,也可自環境溫度升溫至煆燒溫度,並且在煆燒期間維持最終溫度。同樣地,將煆燒後的材料在還原環境(如H2、CO或其混合物,以及惰性氣體)下於約1000℃至約1600℃烘烤一段足夠的時間。或者,還原環境可藉由椰子炭與起始材料分解後的產物反應而產生,藉此將所有煆燒後的材料轉換為所要的磷光體組成物。
雖然上述磷光體組成物可單獨適用於很多應用,但其也可以和一或多種額外的磷光體混合以用在LED光源中。
磷光體組成物可藉由層壓與燒結兩個或多個鑄件帶(cast tapes)以形成陶瓷板來形成,其中鑄件帶可包括任一以化學式I到VIII表示的化合物或其前驅物。美國專利第7,514,721號與美國專利公開號第2009/0108507號揭露層壓與燒結兩個或多個鑄件帶的實例與方法,前述二案的整體內容在此併入本案以供參考。
首先,可選擇性地調整原料(例如基於硝酸鹽或氧化物的原料,如用以形成YAG的Y2O3及Al2O3)的粒子尺寸,以減少溶劑揮發過程中毛細力導致的鑄件帶破裂。例如,可預先退火原料顆粒以得到所欲的粒子尺寸。原料顆
粒可在約800℃到約1800℃的溫度區間(更佳在1000℃到約1500℃)預先退火,以得到所欲的粒子尺寸。預退火可在真空、空氣、O2、H2、H2/N2或稀有氣體(如氦、氬、氪、氙、氡或其組合)下發生。在一實施例中,每一原料都被調整成大約相同的粒子尺寸。在另一實施例中,顆粒具有介於約0.5m2/g到約20m2/g(較佳為約1.0m2/g到約10m2/g,或更佳約3.0m2/g到約6.0m2/g)的BET表面積。
接著,可製備漿液以在之後將其鑄成帶狀。預製的磷光體(例如,以本文描述的流動式(flow-based)熱化學合成方法製備的磷光體)及/或化學計量比的原料可與各種成分混合成混合物。混合物成分的實例包括(但不限於):摻質、分散劑、塑化劑、黏著劑、燒結助劑及溶劑。這些摻質、分散劑、塑化劑、黏著劑、燒結助劑及溶劑可與上述關於成形及燒結製程之說明中所描述者相同。
在一些實施例中,分散劑可選自Flowen、魚油、長鏈高分子、硬脂酸、氧化鯡魚油、雙羧酸(例如丁二酸、失水山梨醇單油酸酯、乙二酸、丙二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、鄰苯二甲酸、對苯二甲酸)及其混合物。
接著,混合物可被粉碎,例如是被球磨一段時間(介於約0.5小時至約100小時,較佳約6小時到48小時,或更佳約12小時到約24小時),以形成漿液。球磨所使用的磨球包括與混合在混合物中的成分不同的材料,例如可為ZrO2。在一實施例中,球磨步驟包括在一段時間後藉過濾
或其他已知隔離方法隔離磨球。在一些實施例中,上述漿液具有介於約10cP到約5000cp(較佳是約100cP到約3000cP,更佳是400cP到1000cP)的黏滯度。
第三,可將漿液澆鑄在釋放基板(releasing substrate,例如塗有矽氧樹脂的聚對苯二甲酸乙二酯基板)上以形成帶件。例如,可使用刮刀將漿液澆鑄在移動式載體上,而後乾燥以形成帶件。鑄件帶的厚度可藉由改變刮刀與移動式載體的間距來調整。在一些實施例中,刮刀與移動式載體的間距在約0.125mm到約1.25mm之間,較佳在約0.25mm到約1.00mm之間,或更佳在約0.375mm到約0.75mm之間。同時,移動式載體的速度是在約10cm/min.到約150cm/min.之間,較佳在約30cm/min.到約100cm/min.之間,或更佳在約40cm/min.到約60cm/min.之間。藉由調整移動式載體的速度和刮刀與移動式載體的間距,帶件可具有介於約20μm至約300μm之間的厚度。澆鑄之後,帶件可選擇性地切成所欲的形狀。
兩或多個帶件可層壓以形成一組件。層壓步驟可包括堆疊兩或多個帶件(例如堆疊2到100個)且使堆疊的帶件受熱及單軸壓力(例如垂直於帶件表面的壓力)。例如,可將堆疊帶件加熱到其所含接著劑的玻璃轉換溫度(Tg)以上,再用金屬模作單軸壓縮。在一些實施例中,單軸壓力在約1MPa到約500MPa之間,較佳在約30MPa到約60MPa之間。在一些實施例中,施加熱與壓力的時間在約1min.到約60min.之間,較佳在約15min.到約45min.之
間,更佳是30min.。層壓步驟可選擇性地包括使用成形模在組件上形成不同的形狀(例如洞或柱)或圖案。
組件的一些實施例包括至少一帶件,其具有由化學式I到VIII中任一者所表示的磷光體組成物。在一些實施例中,所有堆疊的帶件均包括由化學式I到VIII中任一者所表示的磷光體組成物。
可加熱組件以形成複合物。加熱步驟可包括脫脂製程(debinding process)與燒結製程。脫脂製程包括分解至少一部份組件中的有機成分(例如,使組件中的接著劑和塑化劑揮發)。例如,可在空氣中加熱組件到介於約300℃與約1200℃之間的溫度,較佳是介於約500℃到約1000℃之間的溫度,或更佳是800℃。加熱速率是約0.1℃/min.到約10℃/min.,較佳是0.3℃/min.到約5℃/min.,或更佳是約0.5℃/min.到約1.5℃/min.。加熱步驟的實例可更包括在介於約30min.到約300min.之間的一段時間內保持溫度,該段時間的選擇可取決於組件的厚度。
加熱步驟還包括用以形成複合物的燒結製程。可在真空、空氣、氧氣、氫氣、氫/氮氣或鈍氣(例如氦、氬、氪、氙、氡或其組合)中燒結組件。燒結溫度可在約1200℃到約1900℃之間,較佳在約1300℃到約1800℃之間,或更佳在約1350℃到約1700℃之間。燒結時間在約1小時到約100小時之間,較佳在約2小時到約小時之間。在一些實施例中,脫脂製程與燒結製程在單一步驟中完成。
加熱步驟中,可將組件夾於蓋板間以減少其變形(如
撓曲、拱起、彎曲)。蓋板可含特定材料,其溶點高於加熱步驟施加的溫度。此外,蓋板可以多孔得足以使揮發成分穿透而輸送。例如,蓋板可以是孔隙率約40%的二氧化鋯。
磷光體組成物可藉由成形與燒結一或多個磷光體以形成陶瓷板來製備。在一些實施例中,磷光體組成物包括由化學式I到VIII中任一者所表示的組成物。美國專利公開號第2009/0212697號與美國專利申請案第61/315763號揭露陶瓷板與形成陶瓷板的方法的實例,前述二案的整體內容在此併入本案以供參考。
首先提供未加工的磷光體粉末,例如本文描述者,其可使用任何習知或適當的方法來製備,例如本文描述的流動式熱化學合成方法。在一些實施例中,用以形成複合物的磷光體材料的未加工粉末通常是奈米級顆粒,其平均粒徑不大於約1000nm,較佳不大於約500nm,更佳不大於200nm。如粒子尺寸大於約1000nm,可能很難使總透光率高於約50%,因為即使在高溫高壓的燒結條件下,也不易使如此大的顆粒相互融合。如此容易導致許多空隙存留在陶瓷板中。另一方面,奈米級顆粒可以輕易地相互融合,使我們得以製備細緻且無空隙的陶瓷板。原料不需要與磷光體陶瓷板的結果產物具有相同的組成或晶體結構。
在一些實施例中,若有需要,可使用少量助熔劑物質(例如燒結助劑)以改善燒結性質。在一些實施例中,燒結助劑可包括(但不限於)矽酸四乙脂(TEOS)、矽酸膠、
氧化鋰、氧化鈦、氧化鋯、氧化鎂、氧化鋇、氧化鈣、氧化鍶、氧化硼或氟化鈣。其他的燒結助劑包括(但不限於)金屬鹵化物(如NaCl或KCl)及有機化合物(如尿素)。
在一些實施例中,還可包括多種塑化劑以降低玻璃轉換溫度及/或改善陶瓷的可撓性。塑化劑的非限制性實例包括雙羧酸/三羧酸聚酯系列塑化劑,諸如鄰苯二甲酸二(2-乙己基)酯、鄰苯二甲酸二異壬酯、鄰苯二甲酸二正丁酯、鄰苯二甲酸丁酯苯甲酯、鄰苯二甲酸二異癸酯、鄰苯二甲酸二正辛酯、鄰苯二甲酸二異辛酯、鄰苯二甲酸二乙酯、鄰苯二甲酸二異丁酯及鄰苯二甲酸二正己酯;己二酸系列塑化劑,諸如己二酸二(2-乙己基)酯、己二酸二甲酯、己二酸單甲酯及己二酸二辛酯;癸二酸酯系列塑化劑,諸如癸二酸二丁酯;馬來酸酯,諸如馬來酸二丁酯與馬來酸二異丁酯;聚烷基二醇(polyalkylene glycols),諸如聚乙二醇、聚丙二醇及其共聚物;苯甲酸酯;環氧化植物油(epoxidized vegetable oils);磺醯胺,諸如N-乙基甲苯磺醯胺、N-(2-羥丙基)苯磺醯胺及N-丁基苯磺醯胺;有機磷酸酯,諸如磷酸三甲苯酯及磷酸三丁酯;乙二醇/聚醚,如三乙二醇二己酸酯、四乙二醇二庚酸酯;檸檬酸烷酯,諸如檸檬酸三乙酯、乙醯檸檬酸三乙酯、檸檬酸三丁酯、乙醯檸檬酸三丁酯、檸檬酸三辛酯、乙醯檸檬酸三辛酯、檸檬酸三己酯、乙醯檸檬酸三己酯、丁醯檸檬酸三己酯及檸檬酸三甲酯;烷基磺酸苯酯;以及上述材料的組合。
接著可將原料混合且形成成形品。在一些實施例中,
可間或添加黏著樹脂和溶劑於未加工粉末中,使混合與成形製程更容易。黏著劑是可改善組成物(其將被加熱以形成複合物)中顆粒之黏著的任何物質。黏著劑的一些非限制性實例包括聚乙烯醇、聚氯乙烯、聚乙烯丁醛、聚苯乙烯、聚乙二醇、聚乙烯吡咯烷酮、聚醋酸乙烯酯及聚丁酸乙烯酯等等。在一些(但非全部)環境中,黏著劑充分揮發可能有益,因燒結過程裡黏著劑可自前驅混合物中完全移除或消除。可用的溶劑包括(但不限於)水、低級醇(諸如,但不限於變性乙醇、甲醇、異丙醇及其混合物),較佳是變性乙醇、二甲苯、環己酮、丙酮、甲苯、甲乙酮及其混合物。一較佳實施例中,溶劑是二甲苯和乙醇的混合物。
混合製程可藉由研缽與研杵、球磨機、珠磨機或其他等效用具來完成。用於錠成形的簡易模具、熱均壓(HIP)或冷均壓(CIP)均可用於成形製程。在一些實施例中,加入定量的未加工粉末於模中,再施加壓力形成板件。之後以不超過結果之磷光體材料的熔點的高溫燒結成形品。
任何適當的陶瓷燒結方法都可用於製備半透明陶瓷板。在一些實施例中,燒結可在加壓下進行。燒結條件(如溫度曲線、氣體成份、壓力與時間)視磷光體的種類而定。
本文揭露的磷光體組成物可包含於一發光裝置中。本案的範疇涵蓋各種型態的發光裝置。圖1、圖2A與圖2B(未按比例繪製)提供本案範疇所涵蓋的發光裝置的非限制性實例。圖1是具有磷光體粉末組成物的例示發光裝
置。次基板10上裝有光源15,如習知的基底LED。光源15與封裝磷光體粉末20鄰接,其接受至少一部份由光源15放出的光。封裝樹脂25(非必要)置於光源15與封裝磷光體粉末20上。封裝磷光體粉末20可包括本案揭露的任一共摻雜磷光體組成物,例如化學式I的磷光體組成物。
磷光體組成物可封裝在成形體中(例如圖1所繪,封裝於封裝樹脂25中)。例如,可封裝磷光體組成物於樹脂(例如環氧樹脂或矽氧樹脂)中,使其形成成形體。美國專利第5,998,925號與第6,069,440號揭露封裝磷光體的方法與實例,上述兩案的整體內容均在此併入本案以供參考。簡短地說,粉末形式的磷光體組成物可與樹脂混合而形成漿液。接著可硬化此研磨漿液而形成成形體。
在一些實施例中,磷光體組成物與第二磷光體(非必要)混合置於發光裝置中。例如,可製備磷光體組成物(如化學式I)與第二磷光體(例如YAG:Ce)的混合物,然後將其封裝在樹脂中。
圖2A是發光裝置的另一實例,其中磷光體組成物容納於發射層30(例如上述燒結陶瓷板)中,其接受至少一部份由光源15放出的光。發射層30例如可為包括磷光體組成的陶瓷板。在一些實施例中,發射層30包括磷光體組成與非必要的第二磷光體。例如,發射層30可包括磷光體組成(如化學式I)與第二磷光體(例如YAG:Ce)。
圖2B是發光裝置的又一實例,其中磷光體組成物與非必要的第二磷光體容納於分離的發射層中。第一發射層
40置於光源15上,接受至少一部份由光源15放出的光。第一發射層40例如可為包括磷光體組成物及/或非必要的第二磷光體的陶瓷板。第二發射層35置於第一發射層40與光源15之間。第二發射層35也接受至少一部份由光源15放出的光。第二發射層35例如可為包括磷光體組成物及/或非必要的第二磷光體的陶瓷板。在一些實施例中,第一發射層40包括磷光體組成物,第二發射層35包括非必要的第二磷光體。在一些實施例中,第一發射層40包括非必要的第二磷光體,第二發射層35包括磷光體組成物。
圖1、圖2A與圖2B中各部件(如光源、磷光體組成物等)的位置是用以說明,非意欲限制本發明。在一些實施例中,各部件被配置成由磷光體組成物接受至少一部份光源所放射的輻射。在一些實施例中,各部件被配置成由非必要的第二磷光體接受至少一部份光源所放射的輻射。
在一些實施例中,光源(例如圖1、圖2A與圖2B所繪示的光源15)可設成放射藍光輻射。藍光輻射例如可包括介於約430nm與550nm之間的峰值放射波長。在一些實施例中,光源放射具有約450nm的峰值放射波長的藍光輻射。一些實施例包括半導體LED光源。舉例來說,光源可以是與電源連接的AlInGaN基單晶半導體材料。
本案的發光裝置的優勢在可產生寬放射光譜。在一些實施例中,發光裝置放射的輻射可包括介於約500nm與約650nm間的峰值波長。在一些實施例中,磷光體發光裝置放射的輻射可包括介於約515nm與約560nm間的第
一峰值放射波長,以及介於約600nm與約615nm間的第二峰值放射波長。一些實施例中,發光裝置放射的輻射可包括介於約730nm與約770nm間的第三峰值放射波長。
發光裝置還可具有高CRI及/或低CCT,例如可放射CRI至少約70的光。在一些實施例中,CRI至少約80、至少約90或約等於91。參考CCT可在約2500K至約10000K範圍中、在約2500K至約5000K範圍中、在約2500K至約4500K範圍中,或在約2600K至約3400K的範圍中。
本文也揭露產生光的方法,包括將磷光體組成物暴露於藍光輻射。磷光體組成物例如可由化學式I至VIII中任一者表示。在一些實施例中,藍光輻射具有介於約430nm到約550nm的峰值放射波長。在一些實施例中,藍光輻射具有約450nm的峰值放射波長。
本案的方法的優勢在於可產生寬放射光譜。在一些實施例中,此方法產生的輻射可包括介於約500nm與約650nm之間的峰值放射波長。在一些實施例中,此方法產生的輻射可包括介於約515nm與約560nm之間的第一峰值放射波長,以及介於約600nm與約615nm之間的第二峰值放射波長。在一些實施例中,此方法產生的輻射可具有介於約730nm與約770nm之間的第三峰值放射波長。
此方法還可製造具有高CRI及/或低CCT的光,例如CRI至少約70的光。在一些實施例中,CRI至少約80、至少約90或約等於91。參考CCT可在約2500K至約10000
K範圍中、在約2500K至約5000K範圍中、在約2500K至約4500K範圍中,或在約2600K至約3400K的範圍中。
以下實例更詳細揭露額外的實施例,但其並非意欲限制申請專利範圍的範疇。
Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12以下述方法製備:將下列組分(5克Lu2O3、0.345克CeO2、1.055克CaCO3、2.46克Al2O3、0.23克MnCO3及0.755克SiO2)手動混合於甲醇漿液中,直到漿液乾燥。接著將混合物移入氧化鋁舟,並在空氣中以4℃/min.升溫速率加熱至600℃。續於加熱後的混合物上通氫/氮氣,並以4℃/min.加溫速率加溫至1500℃。在1500℃持溫5小時後冷卻至室溫(此時仍曝露在氫/氮氣中)。手動將塊狀物粉碎為粉末,產生Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12(組成物1)以待後續研究。
表1揭露由化學式I表示的組成物的各種實例,其中組成物若於單一欄位中具有一個以上的元素,表示以1:1的莫耳比組合欄位中的每一元素。舉例來說,組成物16具有莫耳比例約相同的鈣與鍶作為主族元素(MG)。組成物2~27是以與上述類似的方法所製備。組成物28~30也可以與上述類似的方法來製備。
以預定強度的標準激發光照射磷光體粉末,並測量其放射現象來評估其發光效率。磷光體的內部量子效率(internal quantum efficiency;IQE)是磷光體產生的光子數目與進入磷光體的激發光的光子數目的比值。
磷光體材料的IQE可由下列公式表示:
外部量子效率(λ)=內部量子效率(λ).[1-R(λ)]
吸收率(λ)=1-R(λ)其中對任何波長λ,E(λ)是入射至磷光體的放射光譜中光子的數目,R(λ)是激發光反射的光譜中光子的數自,而P(λ)是磷光體的放射光譜中光子的數目。IQE的測量方法亦由Ohkubo et al.,"Absolute Fluorescent Quantum Efficiency of NBS Phosphor Standard Samples," 87-93,J.Illum.Eng.Inst.Jpn.Vol.83,No.2,1999所提供,該文的整體揭露內容在此併入本案以供參考。
圖3顯示了組成物1(Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12)的激發光譜,其包括由約390nm到約510nm的相對寬範圍。因此,組成物1可被常用於習知白光LED的藍光(例如約450nm)激發。圖4顯示組成物1受到約450nm的輻射激發的放射光譜。此組成物於約510nm與約600nm有兩個峰值放射波長。
圖5顯示組成物1~9的放射光譜,其中變數x在0.05到0.20間變化。圖5中鈰的百分比例與x值的一半相關。例如,組成物2具有10%的鈰,因此與值為0.20的x相關。在約600nm處的峰值放射隨鈰濃度增加而增加。隨著鈰
濃度增加,峰值也有極小的紅位移。圖6顯示組成物1與組成物10~15的放射光譜,其中錳的百分比例與z值的四分之一相關。例如,組成物10有10%的錳,故與值為0.4的z相關。錳多於4%時,額外峰值出現於750nm附近。
圖7顯示鈰的量變動時的量子效率。測量組成物2~7,其中圖7所示的百分比例與x值的一半相關。增加鈰濃度時,IQE百分比例相對維持不變,而外部量子效率(EQE)與吸收率(Abs.)的百分比率一開始增加,在鈰增加至6%(即x0.12)後維持不變。圖8比較各錳濃度的量子效率。測量組成物1、10、11、14及15,其中圖8所示百分比例與z值的四分之一相關。量子效率大致隨錳量增加而降低。
圖9比較多種主體經改質的組成物的放射光譜。圖9顯示組成物16~22。組成物16~22的IQE分別為52.66%、60.85%,、60.68%、30.16%、35.86%、36.82%及49.74%。當50%的釓或鋱被包含為主體時,在約600nm處的峰值放射提高了,然而這些組成物的IQE比較低。包括50%的鍶、鋇及釔的組成物的IQE約為60%。
圖10比較商用YAG:Ce磷光體(Yttrium Aluminum Garnet,產品編號:BYWO1A/PTCWO1AN,PhosphorTech Corp.,Lithia Springs,GA,USA)與組成物1的放射光譜。與習知YAG:Ce相比,共摻雜磷光體有更寬的放射光譜。
如表2所示,此光譜提供優越的CRI(約91),而YAG:Ce的CRI為71。表2也提供x與y座標,以及色溫。
Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12的磷光體粉末是以感應耦合RF熱電漿熱解製備。將106.287克Lu(NO3)3.6H2O、25.03克Ca(NO3)2.4H2O、182.625克Al(NO3)3.9H2O、5.79克Mn(NO3)2.6H2O、8.686克Ce(NO3)3.6H2O及68.605克22-25%的氨丙基三羥基矽烷(Aminopropylsilane triol)與650克尿素一起溶於約720mL的水中,接著,超音波震盪30分鐘以製備透明的前驅物溶液。使用液體泵浦將0.4M的前驅物溶液經由原子化探針帶入電漿反應腔。
所有的沉積實驗都是以在3.3MHz運作的RF感應電漿炬(TEKNA電漿系統,Inc PL-35)進行。對沉積實驗而言,腔體壓力維持在25kPa至35kPa,而RF產生板功率(plate power)介於10至12kW間。板功率和沉積壓力都是使用者可控制的參數。氬氣經由氣體入口引入電漿炬中,既作為漩渦鞘氣體(swirling sheath gas),也作為中央電漿氣體。鞘氣體流維持在30slm(standard liters per
minute,每分鐘標準升流量),中央氣體流是10slm。
使用放射狀原子化探針(TEKNA電漿系統,Inc SDR-772)注入反應物。注入反應物時,探針置放於電漿捲流(plasma plume)的中心。在沉積過程中,反應物以10ml/min的速率進入電漿捲流。液態反應物的原子化是以氬氣(以流速15slm輸送)作為原子化氣體來進行。如製造商所建議,提供給原子化探針的冷卻水的流速維持在4slm,且壓力維持在1.2MPa。
使用Lu2CaAl4SiO12:Ce,Mn磷光體奈米粉末製備燒結陶瓷板。將4克實例3的方法製備的奈米粉末、0.21克聚(乙烯丁醛-乙烯醇-乙烯乙酸酯)(平均分子量90,000~120,000的粉末,Sigma-Aldrich製)、0.012克燻矽粉末(CAB-O-SIL® HS-5,Cabot公司製)及10ml甲醇以研缽和研杵混合,直到混合物漿液溶液非常滑順。自乾燥器吹送熱空氣並保持研杵移動,使甲醇完全移除而得乾燥粉末。以不同裝入量(45.0、47.5、50.0及52.5mg)將所得乾燥粉末散佈於直徑3mm的模具組(產品號:0012-6646、3mm KBr模具組,International Crystal Laboratories,Inc)中,以液壓機施加4000psi壓力。然後在還原環境(如3%或4%氫氣-97%或96%氮氣的環境)或真空下以管狀爐管(型號GSL 1800X,MTI公司,Richmond,CA,USA)將所得板件在1500℃燒結5小時(加熱速率5℃/min)。所有陶瓷板樣品的晶相經XRD確認為Lu2CaAl4SiO12石榴石。
將實例4的四個陶瓷板裝在藍光LED頂端上,並加2.9V、10mA的直流電於LED。用配備積分球的光感測器(MCPD 7000,Otsuka Electronics,Inc)獲得各樣品的白光光譜。為去除陶瓷板與LED頂端間的空氣間隙,將石蠟油填入間隙。每次量測皆採相同的LED頂端和操作條件。
從這些放射光譜中計算CIE色度(x,y)。表3涵括了陶瓷板以及實例2.5中相同的共摻雜磷光體粉末的結果。陶瓷板的放射光譜顯示在圖11中。為了比較,圖12顯示了實例3的磷光體粉末組成物的放射光譜。
此外也量測樣品之一的總光穿透率,使用的量測系統(MCPD 7000,Otsuka Electronics,Inc,配備Xe燈、單色儀及積分球)與美國專利公開第2009/0212697號描述者相似。以單色儀放射藍光(峰值波長約460nm)激發樣品,並使用相同的光感測器獲得光致發光光譜。Lu2CaAl4SiO12:Ce,Mn陶瓷板的峰值波長約530nm,且在530nm的總光穿透率約為42%。
10‧‧‧次基板
15‧‧‧光源
20‧‧‧封裝磷光體粉末
25‧‧‧封裝樹脂
30‧‧‧發射層
35‧‧‧第二發射層
40‧‧‧第一發射層
圖1顯示含粉末形態磷光體組成物的例示發光裝置。
圖2A與圖2B顯示包括具磷光體組成物的發射層的例
示發光裝置。
圖3為Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12的激發光譜。
圖4顯示受藍光激發時,Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12的放射光譜。
圖5顯示受藍光激發時,具有不同鈰含量的各磷光體組成物的放射光譜。
圖6顯示受藍光激發時,具有不同錳含量的各磷光體組成物的放射光譜。
圖7顯示受藍光激發時,具有不同鈰含量的各磷光體組成物的量子效率。
圖8顯示受藍光激發時,具有不同錳含量的各磷光體組成物的量子效率。
圖9顯示受藍光激發時,具有不同主體晶格的各磷光體組成物的放射光譜。
圖10顯示受藍光激發時,YAG:Ce與(Lu1.92Ce0.08)Ca0.84(Al0.96Mn0.04)4SiO12的放射光譜。
圖11顯示受藍光激發時,具有Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12的燒結陶瓷板的放射光譜。
圖12顯示受藍光激發時,具有Lu2.0Ce0.16Ca0.84Al3.84Mn0.16SiO12的電漿合成粉末的放射光譜。
Claims (39)
- 一種磷光體組成物,包括一化合物,其以化學式(RE2-x+yCexAk1-y)(MG4-z-rSirMnz)(Si1-ePe)O12-rNr表示,其中RE包括至少一稀土金屬;Ak包括至少一鹼土金屬;MG包括至少一主族元素;x大於0且小於等於0.2;y小於1;z大於0且小於等於0.8;e等於0,或小於等於0.16;r等於0,或小於等於1;以及z等於e與y之合。
- 如申請專利範圍第1項所述之磷光體組成物,其中MG是選自由鋁、鈧、銦、鎵、硼、矽及其組合所組成的族群。
- 如申請專利範圍第2項所述之磷光體組成物,其中MG為鋁。
- 如申請專利範圍第1項所述之磷光體組成物,其中RE是選自由鎦、釔、釓、鋱、釤、鐠及其組合所組成的族群。
- 如申請專利範圍第4項所述之磷光體組成物,其中RE為鎦。
- 如申請專利範圍第1項所述之磷光體組成物,其中Ak是選自由鎂、鈣、鋇、鍶及其組合所組成的族群。
- 如申請專利範圍第6項所述之磷光體組成物,其中Ak為鈣。
- 如申請專利範圍第1項所述之磷光體組成物,其中r等於0。
- 如申請專利範圍第1項所述之磷光體組成物,其中e等於0。
- 如申請專利範圍第9項所述之磷光體組成物,其中該化合物是以化學式(Lu2.16-xCex)Ca0.84Al3.84Mn0.16 SiO12表示,其中x大於0.0025且小於0.2。
- 如申請專利範圍第10項所述之磷光體組成物,其中x等於0.16。
- 如申請專利範圍第8項所述之磷光體組成物,其中該化合物是以化學式(Lu1.84+zCe0.16)Ca1-z(Al4-zMnz)SiO12表示,其中z大於0且小於0.8。
- 如申請專利範圍第9或12項所述之磷光體組成物,其中z等於0.04。
- 如申請專利範圍第9或12項所述之磷光體組成物,其中z等於0.02。
- 如申請專利範圍第1項所述之磷光體組成物,其中e大於0。
- 如申請專利範圍第15項所述之磷光體組成物,其中該化合物是以化學式(Lu1.84Ce0.16)Ca(Al4-zMnz)(Si1-zPz)O12表示,其中z至少等於0.01且小於0.16。
- 如申請專利範圍第15或16項所述之磷光體組成物,其中z等於0.02。
- 如申請專利範圍第15或16項所述之磷光體組成物,其中z等於0.04。
- 如申請專利範圍第1項所述之磷光體組成物,其中r大於0.001。
- 如申請專利範圍第19項所述之磷光體組成物,其中e等於0。
- 如申請專利範圍第19或20項所述之磷光體組成物,其中x等於0.16。
- 如申請專利範圍第19項所述之磷光體組成物,其中r等於0.4。
- 如申請專利範圍第19項所述之磷光體組成物,其中r等於1。
- 如申請專利範圍第19項所述之磷光體組成物,其中z等於0.16。
- 如申請專利範圍第1項所述之磷光體組成物,其中該化合物是以選自由(Lu1.86Ce0.16Ca0.98)(Al3.98Mn0.02)SiO12、(Lu1.88Ce0.16Ca0.96)(Al3.96Mn0.04)SiO12、(Lu1.84Ce0.16)Ca(Al3.98Mn0.02)(Si0.98P0.02)O12及(Lu1.84Ce0.16)Ca(Al3.96Mn0.04)(Si0.96P0.04)O12所組成的族群的化學式來表示。
- 如申請專利範圍第1項所述之磷光體組成物,其中 該化合物是以化學式(Lu2-x+zCexCa1-z)(Al4-z-rSirMnz)SiO12-rNr表示,其中:x大於0.001且小於0.4;z大於0.001且小於0.4;以及r大於0.2且小於等於1。
- 如申請專利範圍第26項所述之磷光體組成物,其中該化合物是以選自由(Lu2.0Ce0.16Ca0.84)(Al3.44Si0.40Mn0.16)SiO11.6N0.40以及(Lu2.0Ce0.16Ca0.84)(Al2.84Si1.0Mn0.16)SiO11N1所組成的族群的化學式來表示。
- 如申請專利範圍第1項所述之磷光體組成物,其中該磷光體組成物包括:包括該化合物的微粒。
- 如申請專利範圍第1項所述之磷光體組成物,其中該磷光體組成物是一燒結陶瓷板。
- 如申請專利範圍第1項所述之磷光體組成物,其中當該化合物暴露於具有約450nm波長的輻射時,會放射峰值波長介於約500nm與約650nm之間的輻射。
- 如申請專利範圍第1項所述之磷光體組成物,其中該化合物具有介於約515nm與約560nm之間的第一峰值發射波長,以及介於約600nm與約615nm之間的第二峰值發射波長。
- 一種發光裝置,包括:一光源,用以放射藍光輻射;以及如申請專利範圍第1項所述之磷光體組成物,用以接 收至少一部份的該藍光輻射。
- 如申請專利範圍第32項所述之發光裝置,其中該藍光輻射具有介於約430nm至約550nm之間的峰值發射波長。
- 如申請專利範圍第33項所述之發光裝置,其中該藍光輻射具有約為450nm的峰值發射波長。
- 如申請專利範圍第32~34項中任一項所述之發光裝置,其具有至少為90的演色性指數(color rendering index;CRI)。
- 一種產生光的方法,包括將如申請專利範圍第1項所述之磷光體組成物暴露於藍光輻射下。
- 如申請專利範圍第36項所述之產生光的方法,其中該藍光輻射具有介於約430nm至550nm之間的一峰值發射波長。
- 如申請專利範圍第37項所述之產生光的方法,其中該藍光輻射具有約為450nm的一峰值發射波長。
- 如申請專利範圍第36~38項中任一項所述之產生光的方法,其中該光具有至少為90的演色性指數(CRI)。
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US20140022761A1 (en) * | 2011-01-21 | 2014-01-23 | Osram Sylvania Inc. | Luminescent Converter and LED Light Source Containing Same |
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CN102850047A (zh) * | 2011-06-29 | 2013-01-02 | 圣戈本陶瓷及塑料股份有限公司 | 基于掺杂的镥铝石榴石(LuAG)或其他镥铝氧化物的透明陶瓷闪烁体的制造方法 |
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US9472731B2 (en) * | 2012-12-28 | 2016-10-18 | Shin-Etsu Chemical Co., Ltd. | Phosphor-containing resin molded body, light emitting device, and resin pellet |
CN104232080B (zh) * | 2014-03-25 | 2017-01-11 | 陕西科技大学 | 一种白光led用单一基质全色荧光粉材料及其制备方法 |
US10308175B2 (en) | 2016-09-08 | 2019-06-04 | Ford Global Technologies, Llc | Illumination apparatus for vehicle accessory |
CN106544024B (zh) * | 2016-11-08 | 2019-01-15 | 河北利福光电技术有限公司 | 一种镓铝酸盐荧光粉及其制备方法 |
CN110989242A (zh) * | 2019-12-06 | 2020-04-10 | Tcl华星光电技术有限公司 | 背光模组和显示装置 |
CN112094120A (zh) * | 2020-10-16 | 2020-12-18 | 贵州赛义光电科技有限公司 | 一种发光颜色可调的荧光陶瓷及其制备方法 |
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