CN103400926A - 用于led应用的红光荧光体 - Google Patents
用于led应用的红光荧光体 Download PDFInfo
- Publication number
- CN103400926A CN103400926A CN2013103516559A CN201310351655A CN103400926A CN 103400926 A CN103400926 A CN 103400926A CN 2013103516559 A CN2013103516559 A CN 2013103516559A CN 201310351655 A CN201310351655 A CN 201310351655A CN 103400926 A CN103400926 A CN 103400926A
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- China
- Prior art keywords
- light
- fluorophor
- emitting device
- led
- fluorescent material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
本发明涉及用于LED应用的红光荧光体。本发明还涉及一种发光装置,包括半导体光源以及辐射性连接至所述光源的荧光体材料,荧光体材料包括用Mn4+激活的复合氟化物荧光体。发光器件包括背光源,该背光源具有光源和包括用Mn4+激活的复合氟化物荧光体的荧光体材料,该复合氟化物荧光体可以包括以下中的至少一种:(A)A2[MF5]:Mn4+,其中A选自Li、Na、K、Rb、Cs、NH4及它们的组合;以及其中M选自Al、Ga、In或它们的组合;(B)A3[MF6]:Mn4+:其中A选自Li、Na、K、Rb、Cs、NH4及它们的组合,以及其中M选自Al、Ga、In或它们的组合;(C)Zn2[MF7]:Mn4+,其中M选自Al、Ga、In或它们的组合;以及(D)A[In2F7]:Mn4+,其中A选自Li、Na、K、Rb、Cs、NH4或它们的组合。
Description
本申请是申请日为2008年2月13日,申请号为200880010725.1,发明名称为“用于LED应用的红光荧光体”的发明专利申请的分案申请。
本申请是于2006年2月28日提交的美国专利申请第11/364,611号的部分继续申请并要求其优先权,其又是分别于2005年2月2日和2005年11月11日提交的美国专利申请第11/049,598号和第11/285,442号的部分继续申请。
技术领域
本示例性实施例涉及荧光体组合物,尤其涉及用于发光应用的荧光体。更具体地,本实施例涉及发红光荧光体和采用这些荧光体的发光装置。
背景技术
发光二极管(LED)是通常用作诸如白炽灯的其他光源的替代品的半导体发光体。它们尤其被用作显示灯、报警灯和指示灯或者用在期望得到有色光的其他应用中。由LED产生的光的颜色取决于在LED的制造过程中所使用的半导体材料的类型。
包括发光二极管和激光器(两者在本文中被统称为LED)的有色半导体发光器件已由诸如氮化镓的第III-V族合金制成。对于基于GaN的LED,所发射的光通常在电磁光谱的UV至绿色范围内。直到最近,由于由LED所产生的光的固有颜色,LED已不适合需要明亮白光的发光用应。
近来,已开发了用于将从LED发射的光转换为用于照明的有用光的技术。在一种技术中,LED涂覆或覆盖有荧光体层。荧光体是吸收电磁光谱的一部分中的辐射能量并发射电磁光谱的另一部分中的能量的发光材料。一种重要的荧光体是具有非常高化学纯度和可控组成的结晶无机化合物,其中,该化合物中添加有少量其他成分(被称为“活化剂”)以将其转换为有效的荧光材料。利用活化剂和无机化合物的适当组合,能够控制发光的颜色。最有用和公知荧光体响应于在可见范围外的电磁辐射的激发而发出在电磁光谱的可见部分内的辐射。
通过掺入由LED产生的辐射所激发的荧光体,可以产生例如在光谱的可见范围内的具有不同波长的光。有色LED通常被用在玩具、指示灯和其他装置中。持续的性能改善使其已能够用于在交通灯、出口标志、商店标识等的饱和色的LED的新应用。
除了有色LED之外,LED产生的光和荧光体产生的光的合成可以用于产生白光。最常见的白色LED由发蓝色光的GaInN芯片组成。该发蓝光的芯片涂覆有将一些蓝色辐射转换为互补色(例如,发黄色光)的荧光体。蓝色和黄色辐射一起产生白光。还存在白色LED,其利用近UV发射芯片和包括被设计用于将UV辐射转换为可见光的红色荧光体(红色荧光粉)、绿色荧光体和蓝色荧光体的荧光体混合物。
已知的白光发光器件包括与黄色发光荧光体(诸如,铈(III)掺杂的钇铝石榴石(“YAG:Ce”)、铈(III)掺杂的铽铝石榴石(“TAG:Ce”)或者铕(II)掺杂的原硅酸钡(“BOS”))结合的蓝色发光LED,该蓝色发光LED在近蓝色范围内具有最大发光波长(从约440nm至约480nm)。荧光体吸收从LED发出的辐射的一部分,并将所吸收的辐射转换为黄光。由LED发射的蓝光的其余部分透过荧光体,并与由荧光体发射的黄光混合。观看者将蓝光和黄光混合感知为白光。来自荧光材料和LED芯片的光的总和提供了具有相应的色彩坐标系(x和y)和相关色温(CCT)的色点,并且其光谱分布提供了由显色指数(CRI)衡量的显色能力。
这样的系统可以用于制造具有>4500K的CCT且CRI范围为约72至82的白色光源,其中辐射的发光效能(“LER”,也称为发光度)为约330lm/Wopt。当此范围适合于许多应用时,一般的照明光源通常需要更低的CCT和更高的CRI,优选地,具有类似的或更好的LER。
由蓝色发射芯片和黄色发射荧光体制成的白色LED器件的一种特别优选的应用是用于例如蜂窝式电话、个人数字助理等中的背光源。这些应用需要高CCT值(大于5000K),这容易由上述具有280lm/Wopt或更大的LER值的LED提供。然而,由于黄色荧光体(例如,具有在550nm与610nm之间的最大发射)的使用,所以这些LED的光谱包含在光谱的黄色区域内的过度发射,这大大地降低了背光的色域(color gamut)。
色域是在色度图(例如,CIE1931x,y图)中显示的横跨红色、绿色和蓝色像素的色点之间的区域。用于显示的历史上的“黄金标准”是NTSC色域,其由三组色点坐标(在CIE1931x,y色度图中,红色的x=0.674且y=0.326,绿色的x=0.218且y=0.712,以及蓝色的x=0.140且y=0.080)限定。通常认为,对于许多背光应用而言,大于70%的NTSC的色域可接受的,而对于大多数的任何这样的应用而言,大于90%的NTSC的色域是可接受的。
为了改善使用黄色荧光体的LED背光源的色域,使黄光被过滤,从而减小了LED背光源的有效LER。因此,开发在CCT>5000K处能够提供280lm/Wopt以上的LER而在封装件中不具有黄色荧光体的LED背光源是有益的。红光荧光体特别适用于当与蓝色或近UV LED芯片一起使用时同时获得这样的LER值,如果需要的话,结合至少一种绿色荧光体或蓝色荧光体。
其他白光LED发光系统使用UV或可见光LED芯片与红色、绿色和/或蓝色荧光体的掺和物,该掺和物可以被近UV辐射有效激发以产生白光。
尽管国际上规定了14个标准色样并且能够计算更广的CRI(R1-14)作为它们的平均值,CRI通常被义定为8个标准色样(R1-8)的平均值,通常称为通用显色指数并简称为Ra。具体地,衡量深红色(strong red)的显色的R9值对于应用范围是非常重要的,尤其是医学属性。
随着CCT减小以及/或者CRI增大,LED值通常减小,导致“暖白色”LED的值(CCT<4500K)显著低于那些“冷白色”LED的值(CCT>4500K)。可以通过使用具有线形发射光谱的红色荧光体来提高LER值,这与具有宽带发射的红色荧光体相反。后一种荧光体的发射能量的大部分易于落入人眼的敏感度非常低的光谱的深红色部分,从而减小了LER值。
因此,在许多白光应用中,优选具有线形发射光谱的荧光体(例如,Y2O3:Eu3+)作为红色成分,因为在感兴趣的CCR范围(例如,3000-6500K)内,它使在可接受的CRI值(例如,80-86)处的LER最大化。目前的掺杂有Eu3+的红色荧光灯荧光体不能成功地用在UV LED灯中,因为它们实际上不吸收近UV(370-420nm)光,这导致由于由荧光体带来的散射而引起的不可接受的光损耗。发深红色光的氟氧化物荧光体(例如,3.5MgO*0.5MgF2*GeO2:Mn4+(MFG))可以用在LED灯中,但是由于其发射大多出现在光谱的红色区域内的太远处(超过650nm),所以要考虑对LER的影响。基于掺杂有Mn4+氧化物和卤氧化物主晶格的其他类似荧光体还具有在大于650nm的波长处的主发射峰值。优选地,使用在较低波长(例如,在610至650nm范围内)处具有线形发射最大值的红色荧光体,其在UV至蓝色范围内具有对LED芯片发射的良好吸收性。这在改善LER的同时将通常的CRI维持在80或更高。
因此,对于新的红光荧光体、以及它们与显示高量子效率的UV和可见LED芯片结合使用的掺和物存在持续的需求,从而制造在任何给定CCR处具有高CRI和改善的LER的白光LED以及具有最小黄色发射和高LER的背光源LED。
发明内容
在第一方面,提供了一种包括半导体光源的背光发射器件;其中,背光源包括:峰值发射波长在610nm与650nm之间的红光荧光体;峰值发射波长在510nm与550nm之间的绿光荧光体;以及a)峰值发射波长在440nm与480nm之间的蓝色LED芯片,或者b)峰值发射波长在440nm与480nm之间的蓝光荧光体和具有从约370nm至约440nm的最大发射峰值发射波长的紫色到近UV发射LED芯片。在一种具体实施方式中,用Mn4+激活的复合氟化物荧光体材料被用作红光荧光体。
在第二方面,提供了一种发光器件,包括半导体光源以及用Mn4+激活的复合氟化物荧光体材料。在一个实施例中,该复合氟化物荧光体可以包括以下中的至少一种:(1)A2[MF5]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合;而M选自Al、Ga、In及它们的组合;(2)A3[MF6]:Mn4+:其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合,而M选自Al、Ga、In及它们的组合;(3)Zn2[MF7]:Mn4+,其中,M选自Al、Ga、In及它们的组合;或者(4)A[In2F7]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合。
在第三方面,提供了一种荧光体混合体,包括上述用Mn4+激活的复合氟化物荧光体中的至少一种以及至少一种其他荧光体。
在第四方面,提供了一种荧光体材料,其包括以下中的至少一种:(1)A2[MF5]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合,而M选自Al、Ga、In及它们的组合;(2)A3[MF6]:Mn4+:其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合,而M选自Al、Ga、In及它们的组合;(3)Zn2[MF7]:Mn4+,其中,M选自Al、Ga、In及它们的组合;或者(4)A[In2F7]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合。
附图说明
图1是根据本发明的一个实施例的照明系统的示意性截面图。
图2是根据本发明的第二实施例的照明系统的示意性截面图。
图3是根据本发明的第三实施例的照明系统的示意性截面图。
图4是根据本发明的第四实施例的照明系统的剖面透视图。
图5是根据本发明实施例的K3[AlF6]:Mn4+的激发和发射光谱的曲线图。
图6是使用蓝色芯片与荧光体K2[TiF6]:Mn4+和STG的掺和物的LED的实验性光谱功率分布。
图7是在CIE1931x,y色度图中NTSC标准的色域与LED的色域的曲线表示图,该LED使用蓝色芯片与K2[TiF6]:Mn4+和STG的掺和物。
图8是表面贴装器件(SMD)背光源LED的示意性透视图。
具体实施方式
荧光体将辐射(能量)转换为可见光。荧光体的不同组合提供了不同的有色光发射。本文中提出了新的荧光体组合物和掺和物以及它们在LED和其他光源中的用途。
所产生的可见光的颜色取决于荧光体材料的特定成分。荧光体材料可以仅包括一种荧光体组合物或者包括两种或多种基色荧光体,例如,与黄色和红色荧光体中的一种或多种特定混合以发射期望颜色(色调)的光。如本文中所使用的,术语“荧光体”和“荧光体材料”可以用于表示一种荧光体组合物以及两种或多种荧光体组合物的掺和物。
已确定产生白光的LED灯用于为作为光源的LED赋予期望的质量。因此,在一个实施例中,公开了用于提供白光的由发光材料荧光体转换材料掺和物(荧光体掺和物)涂覆的LED芯片。在此实施例中所提出的荧光体掺和物使得能够在由近UV至绿色LED所发射的从约250nm至550nm的辐射激发时,得到在任何感兴趣的CCT处具有CRI和LER的最佳结合的白光。
参考图1,根据本发明的一种优选结构示出了示例性的基于LED的发光组件或灯10。发光组件10包括半导体UV或可见辐射源,诸如发光二极管(LED)芯片12和电连接至LED芯片的引线14。引线14可以包括由(一个或多个)较厚的引线框支撑的细导线,或者引线可以包括自支撑的电极而省去引线框。引线14为LED芯片12提供电流,并由此使LED芯片12发出辐射。
灯可以包括任何半导体可见光源或UV光源,其能够在其发出的辐射指向荧光体上时产生白光。本发明的LED芯片的优选峰值发射取决于在所披露的实施例中的荧光体的一致性(identity),并且范围可以为从例如250nm-550nm。然而,在一个优选实施例中,LED的发射将在近UV至蓝色-绿色区域内,并且在从约370nm到500nm的范围内具有峰值波长。通常,半导体光源包括掺杂有各种杂质的LED。因此,LED可以包含基于任何合适的III-V、II-VI或IV-IV半导体层并具有约250nm至550nm的峰值发射波长的半导体二极管。
优选地,LED可以包含至少一个半导体层,该半导体层包括GaN、ZnO或SiC。例如,该LED可以包括由式IniGajAlkN(其中,0≤i;0≤j;0≤k,且i+j+k=1)表示的氮化合物半导体,其具有大于约250nm且小于约550nm的峰值发射波长。这样的LED半导体在本领域内是已知的。为了方便,本文中将辐射源描述为LED。然而,如本文中所使用的,术语是指包括所有半导体辐射源,包括例如半导体激光二极管。
虽然在本文中所述的本发明的示例性结构的一般讨论是针对基于无机LED的光源,但是应该理解,除非另外指出,LED芯片可以由有机发光结构或其他辐射源代替,并且当提到任何LED芯片或半导体时仅仅代表任何适当的辐射源。
LED芯片12可以被包封在壳体18内,该壳体将LED芯片和密封剂材料20包封起来。壳体18可以是例如玻璃或塑料。优选地,LED12基本上位于密封剂20的中心。优选地,密封剂20是环氧树脂、塑料、低温玻璃、聚合物、热塑性塑料、热固性材料、树脂或本领域中已知的其他类型的LED封装材料。可选地,密封剂20是旋涂玻璃或具有高折射率的一些其他材料。在一个实施例中,密封剂材料20是聚合物材料,诸如,环氧树脂、硅树脂、或环氧有机硅树脂(silicone epoxy),尽管可以使用其他有机或无机密封剂。优选地,壳体18和密封剂20是透明的或者相对于LED芯片12和荧光体材料22(以下描述)所产生的光的波长基本上是透光的。在一个可替代的实施例中,灯10仅可以包括密封剂材料,而不具有外壳18。LED芯片12可以例如由引线框16、自支撑电极、壳体18的底部、或者由安装于该壳体或引线框的基座(未示出)支撑。
照明系统的结构包括辐射状耦连至LED芯片12的荧光体材料22。辐射状耦连意味着多个元件彼此相联,以使得从一个元件发出的辐射的至少一部分透射至另一个元件。
该荧光体材料22被通过任何适当方法沉积在LED12上。例如,可以形成(一种或多种)荧光体的悬浮液,并且作为荧光体层将其施加于LED表面。在一种这样的方法中,(直接地或者用例如丙酮、MIBK或醋酸丁酯的无机溶剂稀释后)使用硅树脂、环氧树脂或其他基质材料来制造其中荧光体颗粒随机地悬浮并位于LED周围的浆体。该方法仅是对荧光体材料22和LED12的可能位置的示例。因此,可以通过在LED芯片上面涂覆荧光体悬浮液并使其干燥或固化来将荧光体材料22涂覆在LED芯片12的发光面上或直接涂覆在LED芯片12上。壳体18和密封剂20都应该是透明的,以使光24透过那些元件。尽管不是用于限制,但是使用光散射方法或经由显微镜(电子或光学)测量所测量的荧光体材料的中值粒度可以为从约1微米到约20微米。
图2示出了根据本发明的优选方面的系统的第二种优选结构。除非另外说明,图1-图4的对应标号(例如,图1中的12和图2中的112)与每幅图中的对应结构有关。图2的实施例的结构类似于图1的实施例的结构,除了荧光体材料122分散在密封剂材料120内,而不是直接形成在LED芯片112上。荧光体材料(粉末的形式)可以被散分在密封剂材料120的一个区域内,或者更优选地,分布在密封剂材料的整个体积内。由LED芯片112所发出的辐射126与由荧光体材料122所发出的光混合,并且所混合的光表现为白光124。如果荧光体被分散在密封剂材料120内,则可将荧光体粉末加入到装载在LED芯片112周围的聚合物前体中,然后,可以使聚合物前体固化以使聚合物材料凝固。还可以使用其他已知的荧光体分散方法,诸如传递模塑。
图3示出了根据本发明优选方面的系统的第三种优选结构。如3所示的实施例的结构类似于图1的结构,除了荧光体材料222被涂覆到壳体218的表面上,而不是形成在LED芯片212上之外。优选地,该荧光体材料被涂覆在壳体218的内表面上,尽管如果需要的话,荧光体可以被涂覆在壳体的外表面上。荧光体材料222可被涂覆在壳体的整个表面上,或者仅涂覆在壳体的表面的顶部上。由LED芯片212所发出的辐射226与由荧光体材料222所发射的光混合,并且所混合的光表现为白光224。当然,可将图1-图3的结构组合,并且荧光体可以位于任意两个或全部三个位置中,或者任何其他合适的位置中,诸如,与壳体分离或者集成到LED中。
在上述结构的任一种中,灯10还可以包括埋入密封剂材料中的多个散射颗粒(未示出)。该散射颗粒可以包括例如Al2O3颗粒(诸如氧化铝粉)或者TiO2颗粒。散射颗粒有效地使从LED芯片发射的相干光发生散射,优选地具有可忽略的吸收量。
如图4的第四种优选结构中所示,LED芯片412可以被安装在反射杯430中。该杯430可以由反射材料制成或者涂覆有反射材料,诸如,氧化铝、氧化钛或本领域中已知的其他电介质粉末。优选的反射材料为Al2O3。图4的实施例的结构的其余部分与前面的图中任一个的结构的其余部分相同,并且包括两条引线416、将LED芯片412与第二引线电连接的导线432以及密封剂材料420。
另一种优选的结构(特别是用于背光应用)是表面贴装器件(“SMD”)型发光二极管550,例如,如图8所示。此SMD是“侧发射型”,并在导光部件554的突出部分上具有光发射窗552。SMD型发光二极管550可以通过将之前已利用流体焊接等形成的LED放置在玻璃环氧树脂基板上来制成,该玻璃环氧树脂基板上已形成有导电图样并覆盖具有窗552的所述LED。还存在还适合用于本实施例的本领域已知的“顶发射”SMD封装件,例如,Nichia公司制造的SMD封装件。SMD封装件可以包括如上文所限定的LED芯片以及,以下所述的由从LED芯片所发射的光激发的荧光体材料。
在一个实施例中,提供了一种新的荧光体材料,其可以用在上述器件中的荧光体组合物中。该荧光体材料是一种用Mn4+激活的复合氟化物荧光体,并且可以包括以下中的一种或多种:(1)A2[MF5]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合,而M选自Al、Ga、In及它们的组合;(2)A3[MF6]:Mn4+:其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合,而M选自Al、Ga、In及它们的组合;(3)Zn2[MF7]:Mn4+,其中,M选自Al、Ga、In及它们的组合;或者(4)A[In2F7]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合。
在另一个实施例中,另一种非限制性的荧光体组合物是四价配位中心的复合氟化物,例如,A2[MF6]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合,而M选自Ge、Si、Sn、Ti、Zr及它们的组合。
利用“复合氟化物荧光体”,意味着荧光体是一种配位化合物,包含至少一个配位中心(例如,在以上第一种荧光体中的Al),该配位中心围绕着用作配位体的氟化物离子,并且由所需要的抗衡粒子(例如以上实施例中的A)电荷补偿。复合氟化物有时被写成简单的组合、二元氟化物(例如,用3NaF-AlF3代替Na3[AlF6]),但是这种表示法并未示出在配位中心周围的配位体的配位数(在此实施例中,为6)。方括号(有时为了简化而省略)表示它们所包括的复合离子是一种不同于简单氟化物离子的新的化学物质。活化剂离子(Mn4+)还起到配位中心的作用,替代主晶格的中心(例如,Al3+)的一部分。主晶格(包括抗衡离子)还可以改变活化剂离子的激发和发射特性。
当与在250nm至550nm处发射的LED芯片和一种或多种其他荧光体(诸如蓝光荧光体和绿光荧光体)一起使用时,以上荧光体材料的使用可用于白色LED。下文中将更详细地描述与上述荧光体一起使用的其他荧光体。
下表1中详述了此实施例的示例性Mn4+激活的组合物。
表1
ID# | 荧光体 | 原材料 |
1 | K2[AlF5]:Mn2+ | Al(OH)3,K2CO3,K2[MnF6] |
2 | K3[AlF6]:Mn4+ | Al(OH)3,K2CO3,K2[MnF6] |
3 | K3[GaF6]:Mn4+ | Ga2O3,K2CO3,K2[MnF6] |
4 | Zn2[AlF7]:Mn4+ | ZnO,Al(OH)3,K2[MnF6) |
5 | K[In2F7]:Mn4+ | In2O3,K2CO3,K2[MnF6] |
图5示出了K3[AlF6]:Mn4+荧光体的激发和发射光谱。
上述用Mn4+激活的复合氟化物荧光体组合物可以通过以足以确保活化剂离子的所需掺入水平的比率(例如,总M含量的0.1到30mol%之间,更优选地,在2至15mol%之间)采用适当的原材料来制备。在一种示例性制备方法中,将原材料一起溶解于含水氢氟酸中(例如,按重量计30%至50%的HF),而荧光体是通过在塑料或聚四氟乙烯内衬管中将反应混合物蒸发至干燥来制造的,优选在溶液的沸点以下持续加热-例如,在水浴中。然后,可将粗制荧光体磨成期望的粒度(优选为干磨),用有机溶剂(例如,乙醇或丙酮)冲洗以去除任何残余量的HF,并且在空气中干燥后用于LED。
各种其他原始材料可以用于由HF的水溶液和/或其他氟化物(例如,由氧化物、氢氧化物、醇盐、碳酸盐以及金属成分的二元氟化物或氟化氢原位或移位(ex-situ)制备)、以及具有化学计量的量的H2O2或其他过氧化物的高锰酸盐或锰酸盐经由共结晶来制造此实施例中的复合氟化物荧光体,以提供在适当氧化状态的Mn活化剂(+4)。本文中所示的掺杂有Mn4+的复合氟化物荧光体的实例并不是限制性的。在其他组成离子没有引入对用Mn4+激活的荧光体的激发和/或发射有害的电子跃迁或振动跃迁的条件下,它们也可以用于构建复合氟化物主晶格(作为配位中心或抗衡离子)。
在荧光体材料中的每种荧光体的相对量可以根据谱权(spectralweight)来描述。谱权是每种荧光体对荧光体掺和物的整体发射光谱的贡献的相对量。所有单独的荧光体的谱权量总计应该为1。优选的掺和物包含具有从约500nm至610nm的峰值发射的荧光体的从0.01至0.80的谱权、具有从约430nm至500nm的峰值发射的可选荧光体(其不需要利用具有从约430nm至约500nm的峰值发射的蓝色或蓝色-绿色LED的激发)的从0到0.19的谱权、以及上述复合氟化物荧光体中的一种的掺和物的平衡,如实现目标CCT值所需要的。可以使用适合用于近UV到绿色LED系统并在以上波长范围内进行发射的任何已知荧光体。至少用Ce3+激活并且在约500nm至610nm处具有发射最大值的石榴石(例如,本领域中已知的YAG:Ce、TAG:Ce以及它们的组成改性)是尤其优选的荧光体。在后一范围内具有峰值发射的其他特别优选的荧光体是至少用Eu2+激活的碱土金属正硅酸盐,例如,本领域中已知的(Ba,Sr,Ca)2SiO4:Eu2+(“BOS”)及它们的组成改性。
应该注意,本文中描述的各种荧光体中的不同元素被包括在圆括号内并由逗号隔开,诸如,在(Ba,Sr,Ca)2SiO4:Eu2+的情况下。如本领域的技术人员所理解的,这种类型的符号意味着荧光体可以包括任何比率的在化学式中的特定元素中的任何一种或全部。即,例如,以上荧光体的这种类型的符号具有如与(BaaSrbCa1-a-b)2SiO4:Eu2+相同的意义,其中,a和b可以从0到1变化,包括0和1的值。
峰值发射波长在610nm与650nm之间的红光荧光体可以与至少绿光荧光体(例如,具有在510nm与550nm之间的峰值发射波长)以及蓝色LED芯片或蓝光荧光体(例如,具有在440nm与480nm之间峰值发射波长)以及紫色到近UV发射LED芯片(例如,具有从约370nm至约440nm的峰值发射波长)一起用于制备背光源LED。
有利地,实际上用Mn4+激活的任何复合氟化物荧光体都是适合于该红光荧光体的实例。适合的红光荧光体的非限制性实例包括本文中所描述的荧光体、以及在原申请美国专利申请第11/364,611号、第11/049,598号和第11/285,442号中所描述的那些红光荧光体,其全部内容结合于此作为参考。这样的荧光体的特别优选的实例是配位数为6的复合氟化物,例如,A2[MF6]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4及它们的组合;而M选自Ge、Si、Sn、Ti、Zr及它们的组合。适合的绿光荧光体的非限制性实例是碱土金属硫代镓酸盐、硫代铝酸盐或用Eu2+激活的它们的固溶体,例如,用Eu2+激活的硫化镓酸锶(“STG”)SrGa2S4:Eu2+,以及适合的蓝光荧光体的非限制性实例是用Eu2+激活的氯磷酸锶(strontiumchloroapatite)(“SECA”)Sr5(PO4)3Cl:Eu2+。
由用Mn4+激活的复合氟化物荧光体制造的背光源能够具有与典型的蓝色芯片/黄色荧光体LED的LER(例如,在高于5000K的CCT处为大于280lm/Wopt)相等或更好的LER。然而,如之前所说明的,不同于基于黄色荧光体的LED,它们将在不期望用于背光应用的光谱的黄色区域中几乎没有发射。优选地,这样的背光源将具有比NTSC标准的色域大70%的色域,更优选地,在CIE1931x,y图中比NTSC标准大90%。
图6示出了使用蓝色芯片以及荧光体K2[TiF6]:Mn4+和STG的掺和物的LED的实验性光谱。如图7所示,其在CIE1931x,y图中的色度坐标为x=0.315且y=0.335(对应于6300K的CCT)、LER为292lm/Wopt且色域为NTSC的色域的101%。
另外,在基本上不同于本发明中所描述的荧光体的波长的波长处,在整个可见光谱区发射的其他荧光体可以用于掺和物中,以根据用户需求定制所得到的光的白色并制造具有改善的光质量的光源。虽然不是为了进行限制,但是用于具有本荧光体的掺和物中的适合的荧光体包括:
(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+
(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(Sc,Al,Ga)5-αO12-3/2α:Ce3+(其中0≤α≤0.5)
(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;以及
0≤w≤0.2
(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+
ZnS:Cu+,Cl-
ZnS:Cu+,Al3+
ZnS:Ag+,Cl-
ZnS:Ag+,Al3+
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+
掺杂有Eu2+以及/或者Ce3+的(Lu,Ca,Li,Mg,Y)alpha-SiAlON
(Ca,Sr,Ba)SiO2N2:Eu2+,Ce3+
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)
Ca1-σ-x-φCeσ(Li,Na)xEuφAl1+σ-xSi1-σ+xN3,(其中0≤σ≤0.2,0<x≤0.4,0≤φ≤0.2)
对于本申请,应该理解,当荧光体具有两种或多种掺杂剂离子(在以上组合物中在冒号之后的那些离子)时,这意味着该荧光体具有该材料中的那些掺杂剂离子的至少一种(但不一定具有所有的)。即,本领域技术人员应该理解,这种类型的表示方法意味着荧光体可以包括作为化学式中作为的掺杂剂的那些特定离子中的任一种或全部。
当荧光体组合物包括两种或多种荧光体的掺和物时,荧光体掺和物中的每一种荧光体的比率可以根据期望的光输出的特性而变化。可以调整在各个实施例的荧光体掺和物中的各种荧光体的相对比例,以使得当它们的发射被混合并在发光器件中被采用时,制造出在CIE色度图上预定x和y值的可见光。如所述,优选产生白光。例如,该白光的x值范围可以为约0.30至约0.55,以及y值范围可以为约0.30至约0.55。优选地,白光的色点将位于普朗克(也称为黑体)轨迹上或基本上位于其上,例如,在CIE1931色度图的垂直(y)方向上的0.020单位内,更优选地,在垂直方向上的0.010个单位内。然而,若所述,荧光体组合物中的每种荧光体的一致性和量可以根据最终用户的需要而不同。由于供应者提供的各种荧光体的效率在很大幅度上不同,所以所需的每种荧光体的精确量是根据经验来最佳确定的,例如通过标准实验设计(DOE)技术来确定。
可以期望将颜料或滤光材料添加到荧光体组合物中。当LED是UV发射LED时,荧光体层22还可以包含按重量计从0到10%(基于荧光体的总重量)的颜料或能够吸收或反射波长为200nm与450nm之间的UV辐射的其他UV吸收剂材料。
适合的颜料或滤光材料包括能够吸收在200nm与450nm之间产生辐射的本领域中已知的任何颜料或滤光材料。这样的颜料包括例如钛酸镍或锆酸镨。颜料可以以有效过滤在200nm至500nm范围内产生的辐射的10%至100%的量来使用。
实施例
实施例1-K2[AlF5]:Mn4+荧光体的制备
在热板上的特氟龙盘的加热和搅拌条件下将原料(3.52g的Al(OH)3和6.23g的K2CO3)小心地逐渐添加到40ml的50%含水HF中来溶解。将溶液蒸发至干燥,以形成K2[AlF5]主体复合物,接着在加热的条件下边搅拌边将其与0.97g的K2[MnF6]一起溶解于50ml的50%HF中,其中K2[MnF6]是根据Bode方法制备的[H.Bode,H.Jenssen,F.Bandte,Angew.Chem.,N11(1953),304]。将第二种溶液在水浴锅上蒸发至干燥。
实施例2-K3[AlF6]:Mn4+荧光体的制备
对于该荧光体,在热板上的特氟龙盘的加热和搅拌条件下将2.79g的Al(OH)3和7.41g的K2CO3小心地逐渐添加到40ml的50%含水HF中来溶解。将该溶液蒸发至干燥,以形成K3[AlF6]主体复合物,接着与0.77g的K2[MnF6]一起溶解于50ml的50%HF中并在水浴锅上蒸发至干燥。
实施例3-K3[GaF6]:Mn4+荧光体的制备
该制备过程以与前述实施例中相同的方式来进行,在第一步中使用2.91g的Ga2O3和6.43g的K2CO3(溶解于50ml的50%HF中),接着在第二步中使用0.67g的K2[MnF6]。
实施例4-Zn2[AlF7]:Mn4+荧光体的制备
该荧光体是通过将2.57g的Al(OH)3和0.34g的K2[MnF6]溶解到50ml的45%HF中,并且在水浴锅上将该溶液加热到60℃来制备的。然后,缓慢地少量添加5.37g的ZnO,并且将所形成的溶液蒸发至干燥。
实施例5-K[In2F7]:Mn4+荧光体的制备
在水浴锅中边加热边将6.91g的In2O3样品溶解于100ml的50%HF中,然后,逐渐地少量添加3.44g的K2CO3。将溶液在水浴锅上蒸发至干燥,并用100ml乙醇进行沉淀来去除过量的KF,接着进行过滤。收集滤液,蒸发至干燥,并且在加热和搅拌下与0.51g的K2[MnF6]一起溶解于50ml的40%HF中。最终的溶液再次被蒸发至干燥。
除了用于一般照明的白光掺和物,这些荧光体可以单独使用或者用在用于交通信号、标识的LED的掺和物中,并且特别用于LCD背光源应用。对于这些应用而言,具有饱和色的窄红线发射是非常期望的。
除了LED应用之外,上述的荧光体材料还可以用于其他应用中。例如,该材料可以用作荧光灯中、阴极射线管中、等离子体显示装置中或在液晶显示器(LCD)的荧光体。这些应用仅仅是示例性的而不是穷竭的。
已参照各种示例性实施例描述了本发明。当阅读并理解该说明书后会将想到其他变型和改变。本发明旨在包括在所附权利要求及其等同物的范围内的所有这样的变型和改变。
Claims (18)
1.一种发光装置,包括:半导体光源;以及辐射性连接至所述光源的荧光体材料,所述荧光体材料包括用Mn4+激活的复合氟化物荧光体。
2.根据权利要求1所述的发光装置,其中,所述荧光体包括:
A2[MF6]:Mn4+,其中,A选自Li、Na、K、Rb、Cs、NH4、以及它们的组合;而M选自Ge、Si、Sn、Ti、Zr、以及它们的组合。
3.根据权利要求1所述的发光装置,其中,所述光源为发射峰值波长范围为从约370nm至约500nm的辐射的半导体发光二极管(LED)。
4.根据权利要求1所述的发光装置,其中,所述半导体光源包括由化学式IniGajAlkN表示的氮化合物半导体,其中,0≤i,0≤j,0≤k,且i+j+k=1。
5.根据权利要求1所述的发光装置,其中,所述光源为有机发射结构。
6.根据权利要求1所述的发光装置,其中,A是K。
7.根据权利要求1所述的发光装置,还包括包围所述光源和所述荧光体材料的密封剂。
8.根据权利要求1所述的发光装置,其中,所述荧光体材料被分散在所述密封剂中。
9.根据权利要求1所述的发光装置,其中,所述荧光体材料还包括一种或多种其他荧光体。
10.根据权利要求9所述的发光装置,其中,所述一种或多种其他荧光体在430nm至500nm的范围内具有发射最大值。
11.根据权利要求9所述的发光装置,其中,所述一种或多种其他荧光体在500nm至610nm的范围内具有发射最大值。
12.根据权利要求1所述的发光装置,其中,所述发光装置产生白光。
13.根据权利要求12所述的发光装置,其中,所述白光具有小于4500K的CCT。
14.根据权利要求12所述的发光装置,其中,所述白光具有大于90的一般CRI。
15.根据权利要求12所述的发光装置,其中,所述白光具有大于330lm/Wopt的LER。
16.根据权利要求12所述的发光装置,其中,所述白光具有位于普朗克轨迹上或基本位于所述普朗克轨迹上的色点。
17.根据权利要求16所述的发光装置,其中,所述白光的色点位于1931CIE色度图的垂直方向上距所述普朗克轨迹的0.01的范围内。
18.一种荧光体混合体,包括至少一种用Mn4+激活的复合氟化物荧光体和至少一种其他荧光体。
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US10920136B2 (en) | 2015-11-26 | 2021-02-16 | Current Lighting Solutions, Llc | Processes for synthesizing red-emitting phosphors and related red-emitting phosphors |
CN108291142B (zh) * | 2015-11-26 | 2021-03-12 | 卡任特照明解决方案有限责任公司 | 用于合成发红光磷光体的方法以及发红光磷光体 |
CN105505386A (zh) * | 2015-12-16 | 2016-04-20 | 华南理工大学 | 一种Mn4+掺杂的氟铝酸盐红光荧光材料及其制备方法 |
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Also Published As
Publication number | Publication date |
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KR20150046377A (ko) | 2015-04-29 |
US20070205712A1 (en) | 2007-09-06 |
WO2008100517A1 (en) | 2008-08-21 |
CN101646747A (zh) | 2010-02-10 |
KR101731741B1 (ko) | 2017-04-28 |
KR20170048603A (ko) | 2017-05-08 |
CN101646747B (zh) | 2013-09-18 |
CN103400926B (zh) | 2017-12-08 |
KR101623482B1 (ko) | 2016-05-23 |
KR20100015323A (ko) | 2010-02-12 |
US7648649B2 (en) | 2010-01-19 |
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