TWI726878B - 提供改良之鹵化物材料的方法 - Google Patents
提供改良之鹵化物材料的方法 Download PDFInfo
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- TWI726878B TWI726878B TW105113753A TW105113753A TWI726878B TW I726878 B TWI726878 B TW I726878B TW 105113753 A TW105113753 A TW 105113753A TW 105113753 A TW105113753 A TW 105113753A TW I726878 B TWI726878 B TW I726878B
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Abstract
本發明提供一種用於合成顏色穩定之Mn4+摻雜磷光體之方法，其包括使式I、II、III或IV之前驅體在高溫下與呈氣態之含氟氧化劑接觸以形成該顏色穩定之Mn4+摻雜磷光體Aa Bb Cc Dd Xx：Mn4+ (I)
Aai Bbi Cci Dd Xx Yd：Mn4+ (II)
A1 3 G2-m-nMnmMgnLi3F12Op (III)
AZF4：Mn4+ (IV)
其中A為Li、Na、K、Rb、Cs或其組合；B為Be、Mg、Ca、Sr、Ba或其組合；C為Sc、Y、B、Al、Ga、In、Tl或其組合；D為Ti、Zr、Hf、Rf、Si、Ge、Sn、Pb或其組合；X為F或F與Br、Cl及I中之至少一者的組合；Y為O或O與S及Se中之至少一者的組合；A1為Na或K或其組合；G為Al、B、Sc、Fe、Cr、Ti、In或其組合；Z為La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、
Tm、Yb、Lu、Sc、Y、In或其組合；0
a<2；0
b<1；0
c<1；0
d
1；0.8≦ai≦1.2；0.8≦bi≦1.2；0
ci≦1.2；5.0≦x≦7；0.8≦c+d≦1.2；a+2b+3c+4d=x；0.8≦ci+d≦1；5.0≦x+d≦7.0；ai+2bi+3ci+4d=x+2d；0.02
m
0.2；0
n
0.4；且0
Description
Mn4+錯合氟化物磷光體提供具有高功效之高演色性/色域光源之潛在優點。然而，材料對水解或光降解之敏感性可能會限制其在商業產品中之用途。因此，需要改良材料之穩定性。
簡言之，在一個態樣中，本發明係關於一種用於合成顏色穩定之Mn4+摻雜磷光體之方法。使式I、II、III或IV之前驅體在高溫下與呈氣態之含氟氧化劑接觸以形成顏色穩定之Mn4+摻雜磷光體Aa Bb Cc Dd Xx：Mn4+ (I)
Aai Bbi Cci Dd XxYd：Mn4+ (II)
A1 3 G2-m-nMnmMgnLi3F12Op (III)
AZF4：Mn4+ (IV)
其中A為Li、Na、K、Rb、Cs或其組合；B為Be、Mg、Ca、Sr、Ba或其組合；C為Sc、Y、B、Al、Ga、In、Tl或其組合；D為Ti、Zr、Hf、Rf、Si、Ge、Sn、Pb或其組合；X為F或F與Br、Cl及I中之至少一者的組合；Y為O或O與S及Se中之至少一者的組合；A1為Na或K或其組合；
G為Al、B、Sc、Fe、Cr、Ti、In或其組合；Z為La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Sc、Y、In或其組合；0
a<2；0
b<1；0
c<1；0
d
1；0.8≦ai≦1.2；0.8≦bi≦1.2；0
ci≦1.2；5.0≦x≦7；0.8≦c+d≦1.2；a+2b+3c+4d=x；0.8≦ci+d≦1；5.0≦x+d≦7.0；ai+2bi+3ci+4d=x+2d；0.02
m
0.2；0
n
0.4；且0
p<1。
在另一態樣中，本發明係關於可藉由該方法製備之顏色穩定之Mn4+摻雜磷光體，及利用該等磷光體之發光、背光光源及液晶顯示設備。
10‧‧‧發光設備/發光總成/燈
12‧‧‧發光二極體晶片/LED晶片/LED
14‧‧‧引線
16‧‧‧引線框
18‧‧‧外殼
20‧‧‧囊封材料
22‧‧‧磷光體組合物
24‧‧‧白光
112‧‧‧LED晶片
114‧‧‧引線
116‧‧‧引線框
118‧‧‧外殼
120‧‧‧囊封材料
122‧‧‧磷光體組合物/磷光體
124‧‧‧白光
212‧‧‧LED晶片
214‧‧‧引線
216‧‧‧引線框218包殼
220‧‧‧囊封材料
222‧‧‧磷光體組合物
224‧‧‧白光
226‧‧‧輻射
412‧‧‧LED晶片
416‧‧‧引線/第一引線/第二引線
420‧‧‧囊封材料
430‧‧‧反射杯/杯
432‧‧‧導線
550‧‧‧表面安裝裝置型發光二極體
552‧‧‧發光窗
554‧‧‧光導引構件
當參考附圖閱讀以下實施方式時，本發明之此等及其他特徵、態樣及優勢將變得更充分理解，其中在所有圖中，類似字符表示類似部件，其中：
圖1為根據本發明之一個實施例之發光設備的示意性截面視圖；圖2為根據本發明之另一實施例之發光設備的示意性截面視圖；圖3為根據本發明之又一實施例之發光設備的示意性截面視圖；圖4為根據本發明之一個實施例之發光設備的剖開側透視圖；圖5為表面安裝裝置(SMD)背光LED之示意性透視圖。
在根據本發明之方法中，顏色穩定之磷光體的非顏色穩定前驅體在與含有含氟氧化劑之氛圍接觸時退火或經受高溫。非顏色穩定前驅體具有與顏色穩定之磷光體相同或極類似之標稱組成，但其缺乏最終產物之顏色穩定性。
式I之前驅體描述於讓渡給Mitsubishi Chemical Corporation之WO 2014/104143中Aa Bb Cc Dd Xx：Mn4+ (I)
其中A為Li、Na、K、Rb、Cs或其組合；B為Be、Mg、Ca、Sr、Ba或其組合；C為Sc、Y、B、Al、Ga、In、Tl或其組合；D為Ti、Zr、Hf、Rf、Si、Ge、Sn、Pb或其組合；X為F或F與Br、Cl及I中之至少一者的組合；0
a<2；0
b<1；0
c<1；0
d
1；0.8≦c+d≦1.2；5.0≦x≦7；且a+2b+3c+4d=x。
式I之前驅體之實例包括(但不限於)式NaBaAlF6：Mn4+、K2SrAlF6：Mn4+及Na2SrGaF6：Mn4+之化合物。另外的實例及該等化合物之製備揭示於WO 2014/104143中。
式II之前驅體亦描述於WO 2014/104143中Aai Bbi Cci Dd XxYd：Mn4+ (II)
其中Y為O或O與S及Se中之至少一者的組合；0.8≦ai≦1.2 0.8≦bi≦1.2 0
ci≦1.2 0.8≦ci+di≦1 5.0≦x+d≦7.0；ai+2bi+3ci+4d=x+2d；且Y為O或O與S及Se中之至少一者的組合。
式II之前驅體之實例包括(但不限於)式NaBaTiF5O及KCaAl0.5Ti0.5F5.5O0.5之化合物。另外的實例及該等化合物之製備揭示於WO 2014/104143中。
式I及II之前驅體在WO 2014/104143中描述為具有改良之抗水性及減少之隨時間劣化。然而，根據本發明之方法使材料退火甚至可進一步改良諸如抗水性及長期穩定性之特性。
式III之前驅體描述於讓渡給Koninklijke Philips Electronics N.V.之US 2012/0305972中A1 3 G2-m-nMnmMgnLi3F12Op (III)
其中A1為Na或K或其組合；G為Al、B、Sc、Fe、Cr、Ti、In或其組合；
0.02
m
0.2；0
n
0.4；且0
p<1。
式III之前驅體之實例為Na3Al1.94Mn0.03Mg0.03Li3F12。該等前驅體之製備揭示於US 2012/0305972中。
式IV之前驅體描述於讓渡給Fujian Institute of Structure of Matter之CN 102827601中AZF4：Mn4+ (IV)
其中Z為La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Sc、Y、In或其組合。
式IV之前驅體之實例為NaYF4：Mn4+。該等前驅體之製備揭示於CN 102827601中。
儘管本發明者不希望堅持解釋可由使前驅體經受根據本發明之方法引起的顏色穩定性之改良的任何特定理論，但假設前驅體可含有諸如位錯、F-空位、陽離子空位、Mn3+離子、Mn2+離子、OH-替代F-或提供非輻射重組路徑之表面或填隙H+/OH-基團的缺陷，且此等缺陷藉由在高溫下暴露於氧化劑而癒合或移除。
前驅體與含氟氧化劑接觸之溫度可在約200℃至約700℃，尤其在接觸期間約350℃至約600℃，且在一些實施例中約200℃至約700℃之範圍內。在本發明之各種實施例中，溫度為至少100℃、尤其至少225℃且更尤其至少350℃。磷光體前驅體與氧化劑接觸足以將其轉化為顏色穩定之磷光體的時間段。時間及溫度為互相關聯的，且可一起調整，例如增加時間同時降低溫度，或升高溫度同時減少時間。在特定實施例中，時間為至少1小時，尤其至少4小時，更尤其至少6小時，且最尤其至少8小時。在一特定實施例中，前驅體與氧化劑接觸
至少8小時之時間且溫度為至少250℃，例如在約250℃下約4小時且隨後在約350℃之溫度下約4小時。
含氟氧化劑可為F2、HF、SF6、BrF5、NH4HF2、NH4F、KF、AlF3、SbF5、ClF3、BrF3、KrF、XeF2、XeF4、NF3、SiF4、PbF2、ZnF2、SnF2、CdF2或其組合。在特定實施例中，含氟氧化劑為F2。可改變氛圍中氧化劑之量以獲得顏色穩定之磷光體，尤其結合時間及溫度之變化。在含氟氧化劑為F2時，氛圍可包括至少0.5% F2，但在一些實施例中更低濃度可為有效的。特定言之，氛圍可包括至少5% F2，且更尤其至少20% F2。氛圍可另外包括氮氣、氦氣、氖氣、氬氣、氪氣、氙氣與含氟氧化劑之任意組合。在特定實施例中，氛圍由約20% F2及約80%氮氣組成。
前驅體與含氟氧化劑之接觸方式並不至關重要且可以足以將前驅體轉化為具有所需特性之顏色穩定之磷光體的任何方式完成。在一些實施例中，可向含有前驅體之腔室投料，隨後密封以使得當加熱腔室時產生過壓，且在其他實施例中，氟及氮氣混合物在整個退火過程中流動以確保較均勻之壓力。在一些實施例中，可在一段時間之後再引入一額外劑量之含氟氧化劑。
根據本發明之一個實施例之發光設備或發光總成或燈10展示於圖1中。發光設備10包括半導體輻射源，其展示為發光二極體(LED)晶片12，及電連接至LED晶片之引線14。引線14可為由較粗引線框16支撐之細線，或引線可為自支撐電極且引線框可省略。引線14向LED晶片12提供電流且因此使其發射輻射。
燈可包括當所發射輻射引導至磷光體上時能夠產生白光之任何半導體藍色或UV光源。在一個實施例中，半導體光源為摻雜有不同雜質之藍色發光LED。因此，LED可包含基於任何適合III-V、II-VI或IV-IV半導體層且具有約250至550nm發射波長之半導體二極體。特定
言之，LED可含有至少一個包含GaN、ZnSe或SiC之半導體層。舉例而言，LED可包含由式IniGajAlkN(其中0
i；0
j；0
k且i+j+k=1)表示之氮化合物半導體，其具有大於約250nm且小於約550nm之發射波長。在特定實施例中，晶片為具有約400至約500nm峰值發射波長之近uv或藍色發光LED。該等LED半導體為此項技術中已知。為方便起見，輻射源在本文中描述為LED。然而，如本文中所使用，該術語意欲涵蓋所有半導體輻射源，包括例如半導體雷射二極體。此外，儘管本文中論述之本發明例示性結構之一般論述係關於基於無機LED之光源，但應理解，除非另外說明，否則LED晶片可由另一輻射源替換，且對半導體、半導體LED或LED晶片之任何提及僅表示任何適當輻射源，包括(但不限於)有機發光二極體。
在發光設備10中，磷光體組合物22輻射耦接至LED晶片12。輻射耦接意謂元件彼此結合以使得輻射自一個元件透射至另一元件。藉由任何適當方法使磷光體組合物22沈積於LED 12上。舉例而言，可形成磷光體之水基懸浮液，且將其以磷光層形式塗覆至LED表面上。在一種該方法中，將磷光粒子隨機懸浮之聚矽氧漿液置放於LED周圍。此方法僅為磷光體組合物22及LED 12之可能位置的實例。因此，可藉由在LED晶片12上塗佈磷光體懸浮液且將其乾燥而將磷光體組合物22塗佈於LED晶片12上或直接塗佈於LED晶片12之發光表面上。在基於聚矽氧之懸浮液的情況下，使懸浮液在適當溫度下固化。外殼18及囊封材料20均應為透明的以允許白光24透過彼等元件。儘管並不意欲限制，但在一些實施例中，磷光體組合物之中值粒度在約1至約50微米、尤其約15至約35微米範圍內。
在其他實施例中，磷光體組合物22係散佈於囊封材料20內，而非直接形成於LED晶片12上。磷光體(呈粉末形式)可散佈於囊封材料20之單個區域內或在囊封材料之整個體積中。由LED晶片12發射之藍
光與由磷光體組合物22發射之光混合，且混合之光呈現為白光。若磷光體散佈於囊封材料20內，則可將磷光體粉末添加至聚合物或聚矽氧前驅體，裝載於LED晶片12周圍，且隨後可使聚合物前驅體固化以使聚合物或聚矽氧材料凝固。亦可使用其他已知磷光體散佈方法，諸如轉移裝載。
在一些實施例中，囊封材料20為具有折射率R之聚矽氧基質，且除磷光體組合物22以外，含有具有小於約5%吸光度及R±0.1之折射率的稀釋劑材料。稀釋劑材料具有
1.7、尤其
1.6且更尤其
1.5之折射率。在特定實施例中，稀釋劑材料具有式II，且具有約1.4之折射率。將光學非活性材料添加至磷光體/聚矽氧混合物可產生光通量穿過磷光體/囊封混合物之較漸進分佈且可對磷光體產生較少破壞。稀釋劑之適合材料包括折射率在約1.38(AlF3及K2NaAlF6)至約1.43(CaF2)範圍內之氟化物，諸如LiF、MgF2、CaF2、SrF2、AlF3、K2NaAlF6、KMgF3、CaLiAlF6、K2LiAlF6及K2SiF6，及折射率在約1.254至約1.7範圍內之聚合物。適用作稀釋劑之聚合物之非限制性實例包括聚碳酸酯；聚酯；耐綸；聚醚醯亞胺；聚醚酮；及衍生自苯乙烯、丙烯酸酯、甲基丙烯酸脂、乙烯基、乙酸乙烯酯、乙烯、氧化丙烯及氧化乙烯單體之聚合物；及其共聚物，包括鹵化及未鹵化衍生物。可在聚矽氧固化之前將此等聚合物粉末直接併入聚矽氧囊封材料中。
在又一實施例中，磷光體組合物22塗佈至外殼18之表面上，而非形成於LED晶片12上。磷光體組合物較佳塗佈於外殼18之內表面上，但必要時磷光體可塗佈於外殼之外表面上。磷光體組合物22可塗佈於外殼之整個表面或僅外殼表面之頂部上。由LED晶片12發射之UV/藍光與由磷光體組合物22發射之光混合，且混合之光呈現為白光。當然，磷光體可位於任兩個或所有三個位置中或任何其他適合位置中，諸如與外殼分開或整合至LED中。
圖2說明根據本發明之系統之第二結構。除非另外說明，否則圖1-4之對應數字(例如圖1中之12及圖2中之112)係關於各圖中之對應結構。圖2之實施例的結構類似於圖1之結構，但其中磷光體組合物122係散佈於囊封材料120內，而非直接形成於LED晶片112上。磷光體(呈粉末形式)可散佈於囊封材料之單個區域內或在囊封材料之整個體積中。由LED晶片112發射之輻射(由箭頭126指示)與由磷光體122發射之光混合，且混合之光呈現為白光124。若欲將磷光體散佈於囊封材料120內，則可將磷光體粉末添加至聚合物前驅體，且裝載於LED晶片112周圍。隨後可使聚合物或聚矽氧前驅體固化以使聚合物或聚矽氧凝固。亦可使用其他已知的磷光體散佈方法，諸如轉移成型。
圖3說明根據本發明之系統之第三可能結構。圖3中所示之實施例的結構類似於圖1之結構，但其中磷光體組合物222係塗佈至包殼218之表面上，而非形成於LED晶片212上。磷光體組合物222較佳塗佈於包殼218之內表面上，但必要時磷光體可塗佈於包殼之外表面上。磷光體組合物222可塗佈於包殼之整個表面或僅包殼表面之頂部上。由LED晶片212發射之輻射226與由磷光體組合物222發射之光混合，且混合之光呈現為白光224。當然，可組合圖1-3之結構，且磷光體可位於任兩個或所有三個位置中或任何其他適合位置中，諸如與包殼分開或整合至LED內。
在上述結構中之任一者中，燈亦可包括複數個嵌入囊封材料中之散射粒子(未示)。散射粒子可包含例如氧化鋁或二氧化鈦。散射粒子有效散射自LED晶片發射之定向光，其較佳具有可忽略量之吸收。
如圖4中之第四結構中所示，LED晶片412可安裝於反射杯430中。杯430可由介電材料製成或塗佈有介電材料，諸如氧化鋁、二氧化鈦或此項技術中已知的其他介電質粉末，或由諸如鋁或銀之反射金屬塗佈。圖4之實施例之結構的其餘部分與先前圖式中之任一者的部
分相同，且可包括兩個引線416、導線432及囊封材料420。反射杯430由第一引線416支撐，且導線432用以將LED晶片412與第二引線416電連接。
另一結構(尤其用於背光應用)為表面安裝裝置(「SMD」)型發光二極體550，例如如圖5中所說明。此SMD為「側發射型」且在光導引構件554之突出部分上具有發光窗552。SMD封裝可包含如上文所定義之LED晶片及由自LED晶片發射之光激發的磷光材料。在其他實施例中，圖1-4之LED燈可用作安置於液晶面板之背表面上的背光光源設備。具有包括半導體光源；及根據本發明的顏色穩定之Mn4+摻雜磷光體之顯示器的裝置包括(但不限於)TV、電腦、智慧型電話、平板電腦及其他手持型裝置。
當用於在350至550nm下發射之LED及一或多種其他適當磷光體時，所得發光系統將產生具有白色之光。燈10亦可包括嵌入囊封材料中之散射粒子(未示)。散射粒子可包含例如氧化鋁或二氧化鈦。散射粒子有效散射自LED晶片發射之定向光，其較佳具有可忽略量之吸收。
除顏色穩定之Mn4+摻雜磷光體以外，磷光體組合物22可包括一或多種其他磷光體。當用於發光設備與發射約250至550nm範圍內之輻射的藍色或近UV LED之組合中時，由總成發射之所得光將為白光。其他磷光體，諸如綠色、藍色、黃色、紅色、橙色或其他顏色磷光體可用於摻合物中以定製所得光之白色且產生特定光譜功率分佈。任何所需顏色之量子點亦可用於磷光體組合物22，或可安置於與磷光體組合物22分開之層中。適用於磷光體組合物22中之其他材料包括電致發光聚合物，諸如聚茀，較佳聚(9,9-二辛基茀)及其共聚物，諸如聚(9,9'-二辛基茀-共-雙-N,N'-(4-丁基苯基)二苯胺)(F8-TFB)；聚(乙烯基咔唑)及聚伸苯基伸乙烯基及其衍生物。此外，發光層可包括藍
色、黃色、橙色、綠色或紅色磷光染料或金屬錯合物或其組合。適用作磷光染料之材料包括(但不限於)參(1-苯基異喹啉)銥(III)(紅色染料)、參(2-苯基吡啶)銥(綠色染料)及雙(2-(4,6-二氟苯基)吡啶根基-N,C2)銥(III)(藍色染料)。亦可使用來自ADS(American Dyes Source,Inc.)之市售螢光及磷光金屬錯合物。ADS綠色染料包括ADS060GE、ADS061GE、ADS063GE及ADS066GE、ADS078GE及ADS090GE。ADS藍色染料包括ADS064BE、ADS065BE及ADS070BE。ADS紅色染料包括ADS067RE、ADS068RE、ADS069RE、ADS075RE、ADS076RE、ADS067RE及ADS077RE。
適用於磷光體組合物22之磷光體包括(但不限於)：((Sr1-z(Ca,Ba,Mg,Zn)z)1-(x+w)(Li,Na,K,Rb)wCew)3(Al1-ySiy)O4+y+3(x-w)F1-y-3(x-w)，0<x
0.10，0
y
0.5，0
z
0.5，0
w
x；(Ca,Ce)3Sc2Si3O12(CaSiG)；(Sr,Ca,Ba)3Al1-xSixO4+xF1-x：Ce3+(SASOF))；(Ba,Sr,Ca)5(PO4)3(Cl,F,Br,OH)：Eu2+,Mn2+；(Ba,Sr,Ca)BPO5：Eu2+,Mn2+；(Sr,Ca)10(PO4)6*vB2O3：Eu2+(其中0<v 
1)；Sr2Si3O8*2SrCl2：Eu2+；(Ca,Sr,Ba)3MgSi2O8：Eu2+,Mn2+；BaAl8O13：Eu2+；2SrO*0.84P2O5*0.16B2O3：Eu2+；(Ba,Sr,Ca)MgAl10O17：Eu2+,Mn2+；(Ba,Sr,Ca)Al2O4：Eu2+；(Y,Gd,Lu,Sc,La)BO3：Ce3+,Tb3+；ZnS：Cu+,Cl-；ZnS：Cu+,Al3+；ZnS：Ag+,Cl-；ZnS：Ag+,Al3+；(Ba,Sr,Ca)2Si1-ξO4-2ξ：Eu2+(其中0
ξ
0.2)；(Ba,Sr,Ca)2(Mg,Zn)Si2O7：Eu2+；(Sr,Ca,Ba)(Al,Ga,In)2S4：Eu2+；(Y,Gd,Tb,La,Sm,Pr,Lu)3(Al,Ga)5-αO12-3/2α：Ce3+(其中0
α
0.5)；(Ca,Sr)8(Mg,Zn)(SiO4)4Cl2：Eu2+,Mn2+；Na2Gd2B2O7：Ce3+,Tb3+；(Sr,Ca,Ba,Mg,Zn)2P2O7：Eu2+,Mn2+；(Gd,Y,Lu,La)2O3：Eu3+,Bi3+；(Gd,Y,Lu,La)2O2S：Eu3+,Bi3+；(Gd,Y,Lu,La)VO4：Eu3+,Bi3+；(Ca,Sr)S：Eu2+,Ce3+；SrY2S4：Eu2+；CaLa2S4：Ce3+；(Ba,Sr,Ca)MgP2O7：Eu2+,Mn2+；
(Y,Lu)2WO6：Eu3+,Mo6+；(Ba,Sr,Ca)βSiγNμ：Eu2+(其中2β+4γ=3μ)；Ca3(SiO4)Cl2：Eu2+；(Lu,Sc,Y,Tb)2-u-vCevCa1+uLiwMg2-wPw(Si,Ge)3-wO12-u/2(其中-0.5
u
1，0<v
0.1，且0
w
0.2)；(Y,Lu,Gd)2-φCaφSi4N6+φC1-φ：Ce3+(其中0
φ
0.5)；摻雜有Eu2+及/或Ce3+之(Lu,Ca,Li,Mg,Y),α-SiAlON；(Ca,Sr,Ba)SiO2N2：Eu2+,Ce3+；β-SiAlON：Eu2+,3.5MgO*0.5MgF2*GeO2：Mn4+；Ca1-c-fCecEufAl1+cSi1-cN3(其中0
c
0.2，0
f
0.2)；Ca1-h-rCehEurAl1-h(Mg,Zn)hSiN3(其中0
h
0.2，0
r
0.2)；Ca1-2s-tCes(Li,Na)sEutAlSiN3(其中0
s
0.2，0
f
0.2，s+t>0)；(Sr,Ca)AlSiN3：Eu2+；及Ca1-σ-χ-ΦCeσ(Li,Na)χEuΦAl1+σ-χSi1-σ+χN3(其中0
σ
0.2，0
χ
0.4，0
Φ
0.2)。
磷光體摻合物中個別磷光體中每一者之比率可視所需光輸出之特徵而變化。可調整各種實施例磷光體摻合物中個別磷光體的相對比例，以使得當其發射摻合且用於LED發光裝置中時，在CIE色度圖表上產生預定x及y值之可見光。如所述，較佳產生白光。此白光可例如具有在約0.20至約0.55範圍內之x值及在約0.20至約0.55範圍內之y值。如所述，然而，磷光體組合物中各磷光體之確切身分及量可根據最終使用者之需求而變化。舉例而言，可將材料用於意欲供液晶顯示器(LCD)背光用之LED。在此應用中，基於通過LCD/濾色器組合之後的所需白色、紅色、綠色及藍色適當調諧LED色點。
本發明之色彩穩定Mn4+摻雜磷光體可用於除上文所述之應用外的應用。舉例而言，該材料可用作螢光燈、陰極射線管、電漿顯示裝置或液晶顯示器(LCD)中之磷光體。該材料亦可用作電磁量熱計、γ射線攝影機、電腦斷層攝影術掃描儀或雷射中之閃爍器。此等用途僅為例示性而非限制性的。
實例1
將Na2Ba0.5AlFe：Mn4+之樣品置放於爐室中。將爐室使用機械泵抽
空且用氮氣及氮氣、氟混合物吹掃多次。在數個泵吸及吹掃循環之後，爐室填充有含有20%氟氣及80%氮氣之氛圍，達至約一個大氣壓之壓力。隨後將腔室加熱至約540℃。在保持約12小時之後，將腔室冷卻至室溫。抽空氟氮混合物，將腔室用氮氣填充且吹掃數次以確保在打開腔室之前完全移除氟氣。
實例2
將NaBaTiF5O：Mn4+之樣品置放於爐室中。將爐室使用機械泵抽空且用氮氣及氮氣、氟混合物吹掃多次。在數個泵吸及吹掃循環之後，爐室填充有含有20%氟氣及80%氮氣之氛圍，達至約一個大氣壓之壓力。隨後將腔室加熱至約500℃。在保持約4小時之後，將腔室冷卻至室溫。抽空氟氮混合物，將腔室用氮氣填充且吹掃數次以確保在打開腔室之前完全移除氟氣。
雖然本文中僅已說明且描述本發明之某些特徵，但熟習此項技術者應想到諸多修改及變化。因此，應理解，隨附申請專利範圍意欲將所有該等修改及變化涵蓋為屬於本發明之真實精神內。
10‧‧‧發光設備/發光總成/燈
12‧‧‧發光二極體晶片/LED晶片/LED
14‧‧‧引線
16‧‧‧引線框
18‧‧‧外殼
20‧‧‧囊封材料
22‧‧‧磷光體組合物
24‧‧‧白光
Claims (14)
- 一種用於合成顏色穩定之Mn4+摻雜磷光體之方法，該方法包含使式I、II或III之前驅體AaBbCcDdXx：Mn4+ (I) AaiBbiCciDdXxYd：Mn4+ (II) A1 3G2-m-nMnmMgnLi3F12-pOp (III)在高溫下與呈氣態之含氟氧化劑接觸以形成該顏色穩定之Mn4+摻雜磷光體；其中A為Li、Na、K、Rb、Cs或其組合；B為Be、Mg、Ca、Sr、Ba或其組合；C為Sc、Y、B、Al、Ga、In、Tl或其組合；D為Ti、Zr、Hf、Rf、Si、Ge、Sn、Pb或其組合；X為F或F與Br、Cl及I中之至少一者的組合；Y為O或O與S及Se中之至少一者的組合；A1為Na或K或其組合；G為Al、B、Sc、Fe、Cr、Ti、In或其組合；0a<2；0
b<1；0
c<1；0
d
1；0.8≦ai≦1.2；0.8≦bi≦1.2；0
ci≦1.2；5.0≦x≦7； 0.8≦c+d≦1.2；a+2b+3c+4d=x；0.8≦ci+d≦1；5.0≦x+d≦7.0；ai+2bi+3ci+4d=x+2d；0.02
m
0.2；0
n
0.4；且0
p<1。
- 如請求項1之方法，其中該前驅體具有式I。
- 如請求項1之方法，其中該前驅體具有式II。
- 如請求項1之方法，其中該前驅體具有式III。
- 如請求項1之方法，其中X為F。
- 如請求項1之方法，其中Y為O。
- 如請求項1之方法，其中B為Ca、Sr、Ba或其組合。
- 如請求項1之方法，其中C為Al、Ga或其組合。
- 如請求項1之方法，其中D為Si、Ge、Ti或其組合。
- 如請求項1之方法，其中該含氟氧化劑為F2。
- 如請求項1之方法，其中該溫度係在約200℃至約700℃之範圍內。
- 一種用於合成顏色穩定之Mn4+摻雜磷光體的方法，該方法包含使式I之前驅體在高溫下與呈氣態之含氟氧化劑接觸以形成該顏色穩定之Mn4+摻雜磷光體AaBbCcDdXx：Mn4+ (I)其中A為Li、Na、K、Rb、Cs或其組合；B為Be、Mg、Ca、Sr、Ba或其組合； C為Sc、Y、B、Al、Ga、In、Tl或其組合；D為Ti、Zr、Hf、Rf、Si、Ge、Sn、Pb或其組合；X為F或F與Br、Cl及I中之至少一者的組合；0a<2；0
b<1；0
c<1；0
d
1；0.8≦c+d≦1.2；5.0≦x≦7；且a+2b+3c+4d=x。
- 一種用於合成顏色穩定之Mn4+摻雜磷光體的方法，該方法包含使式II之前驅體在高溫下與呈氣態之含氟氧化劑接觸以形成該顏色穩定之Mn4+摻雜磷光體AaiBbiCciDdXxYd：Mn4+ (II)其中A為Li、Na、K、Rb、Cs或其組合；B為Be、Mg、Ca、Sr、Ba或其組合；C為Sc、Y、B、Al、Ga、In、Tl或其組合；D為Ti、Zr、Hf、Rf、Si、Ge、Sn、Pb或其組合；X為F或F與Br、Cl及I中之至少一者的組合；Y為O或O與S及Se中之至少一者的組合；0.8≦ai≦1.2；0.8≦bi≦1.2；0ci≦1.2；0
d
1；5.0≦x≦7； 0.8≦ci+d≦1；5.0≦x+d≦7.0；且ai+2bi+3ci+4d=x+2d。
- 一種用於合成顏色穩定之Mn4+摻雜磷光體的方法，該方法包含使式III之前驅體在高溫下與呈氣態之含氟氧化劑接觸以形成該顏色穩定之Mn4+摻雜磷光體A1 3G2-m-nMnmMgnLi3F12Op (III)其中A1為Na或K或其組合；G為Al、B、Sc、Fe、Cr、Ti、In或其組合；0.02m
0.2；0
n
0.4；且0
p<1。
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| US10193030B2 (en) | 2016-08-08 | 2019-01-29 | General Electric Company | Composite materials having red emitting phosphors |
| WO2018190827A1 (en) * | 2017-04-12 | 2018-10-18 | General Electric Company | Devices containing a remote phosphor package with red line emitting phosphors and green emitting quantum dots |
| DE102017123265B4 (de) * | 2017-10-06 | 2023-05-11 | OSRAM Opto Semiconductors Gesellschaft mit beschränkter Haftung | Leuchtstoff und Konversions-LED |
| DE102017123269A1 (de) * | 2017-10-06 | 2019-04-11 | Osram Opto Semiconductors Gmbh | Leuchtstoff und Konversions-LED |
| CN107706403B (zh) * | 2017-11-20 | 2020-09-25 | 中国科学院过程工程研究所 | 一种复合碳材料及采用其制备的改性电极材料和锂离子电池 |
| CN109280551B (zh) * | 2018-10-23 | 2019-07-12 | 旭宇光电（深圳）股份有限公司 | 高光效的氟氧化物荧光粉及其制备方法和半导体发光装置 |
| CN109294566A (zh) * | 2018-10-29 | 2019-02-01 | 温州大学 | 一种四价锰离子激活的氟铟酸钡红色荧光粉及其制备方法 |
| CN110684527B (zh) * | 2019-07-24 | 2022-07-12 | 云南民族大学 | 一种蓝光激发的掺Mn4+的六氟铁酸盐红色发光材料及其合成方法 |
| CN112816467B (zh) * | 2021-02-08 | 2023-08-29 | 杭州可靠护理用品股份有限公司 | 一种用于尿液检测的显色剂及其在纸尿裤上的应用 |
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| WO2014152787A1 (en) * | 2013-03-15 | 2014-09-25 | General Electric Company | Color stable red-emitting phosphors |
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| Publication number | Publication date |
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| JP2018518559A (ja) | 2018-07-12 |
| KR20180008689A (ko) | 2018-01-24 |
| TW201708502A (zh) | 2017-03-01 |
| WO2016186636A1 (en) | 2016-11-24 |
| CN107592880A (zh) | 2018-01-16 |
| JP6704001B2 (ja) | 2020-06-03 |
| MY185717A (en) | 2021-05-31 |
| EP3298103A1 (en) | 2018-03-28 |
| US20180155618A1 (en) | 2018-06-07 |
| KR102167629B1 (ko) | 2020-10-20 |
| US10954438B2 (en) | 2021-03-23 |
| EP3298103B1 (en) | 2019-09-04 |
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