CN101663371B - 具有改进的颜色稳定性的白色发光光源和发光材料 - Google Patents

具有改进的颜色稳定性的白色发光光源和发光材料 Download PDF

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CN101663371B
CN101663371B CN2008800127753A CN200880012775A CN101663371B CN 101663371 B CN101663371 B CN 101663371B CN 2008800127753 A CN2008800127753 A CN 2008800127753A CN 200880012775 A CN200880012775 A CN 200880012775A CN 101663371 B CN101663371 B CN 101663371B
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lighting system
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luminescent material
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J·迈耶
H·贝克特尔
W·迈尔
P·施米特
B·-S·斯雷尼马彻
D·U·韦彻特
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Abstract

本发明涉及一种具有改进的发光材料的白色发光光源，该发光材料的通式为(AEN2/3)*b(MN)*c(SiN4/3)*d1 CeO3/2*d2 EuO*x SiO2*yAlO3/2，其中AE为选自Ca、Mg、Sr和Ba或其混合物的碱土金属，且M为选自Al、B、Ga、Sc或其混合物的三价元素，d1＞10*d2。对于宽范围的应用而言，这一材料与产生紫外到蓝光的装置结合，使得可获得改进的光质量和稳定性，特别是改进的温度稳定性。

Description

具有改进的颜色稳定性的白色发光光源和发光材料
技术领域
本发明涉及用于发光装置的新颖发光材料，具体涉及用于LED的新颖发光材料领域。
背景技术
对于照明目的，高CRI光源通常是优选的。基于单一YAG:Ce发光颜色转换器的白色LED一般Ra值达到七十几，在红色光谱区域内具有非常差的显色。因此，对在整个可见光谱区域上具有出色显色的高效照明级白色LED的发展有着迫切要求。改善显色的显而易见的措施是添加红色发光材料(即，披露于US6717353)。然而，由于自由度增加，白色LED的制作变得更加麻烦。因此，即使可能不是最优的，单一磷光体选择被认为是有利的。
然而，对于这样的新颖发光材料仍存在持续的需求，该发光材料在大范围应用中可以使用且特别是使得可以制作具有低于6000K相关色温、优化流明效率和显色的白色磷光体转换LED(pcLED)。
发明内容
本发明的目的是提供一种照明系统，其在大范围应用中可以使用且特别是使得可以制作具有优化流明效率和显色的暖白色pcLED。
这一目的是通过如本发明权利要求1所述的照明系统来实现。相应地，提出一种照明系统，其包括成份大致如下的至少一种发光材料：
a(AEN2/3)*b(MN)*c(SiN4/3)*d1 CeO3/2*d2 EuO*x SiO2*yAlO3/2
其中AE为选自Ca、Mg、Sr和Ba或其混合物的碱土金属，且M为选自Al、B、Ga、Sc或其混合物的三价元素，
其中
0.95≤2*(a+d1+d2)/(b+c+x+y)≤1.2
a+d1+d2≥c+x，
(b+y)∶(c+x)≥1，
(b+y)≤1+10*d1，
b≥5*y，
c≥10*x，
0.0001≤d1≤0.2和d1≥10*d2。
措辞“大致上”具体指≥95％，优选地≥97％且最优选地≥99％的重量％。然而，在一些应用中，痕量的添加剂也可以存在于总成份内。这些添加剂具体地包括本领域中已知为焊剂的物质。合适的焊剂包括碱土金属或碱金属氧化物、氟化物、SiON、SiAlON、SiO2等及其混合物。
对于本发明内的宽范围应用，这一照明系统已经显示出具有至少一个下述优点：
-照明系统的颜色控制可以大幅提高，因为对于本发明内的宽范围应用，激励源的蓝色波长的变化被转换层内的光谱偏移补偿。
-不依赖于用于本发明内的宽范围应用的激励波长，可以达到色度图的黑体线上总体上非常相似的色点。
-本发明的发光材料表现出发光效率的出色的热和光热稳定性，这与上述优点结合，得到高度温度稳定的照明系统。
-此外，本发明的发光材料在宽光谱范围上强烈吸收近紫外到蓝光，因此其可以与各种光源一起使用。
-该材料的特殊属性在于其能够产生具有由材料成份决定的不同蓝色发射波长的窄色温范围。
根据本发明优选实施例，
0.97≤2*(a+d1+d2)/(b+c+x+y)≤1.15，优选地，1≤2*(a+d1+d2)/(b+c+x+y)≤1.10。已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
根据本发明优选实施例，d1≥10*d2，优选地d1≥20*d2，更优选d1≥30*d2以及最优选d1≥40*d2。
已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
根据本发明优选实施例，铈掺杂级d1≥a的0.01％且≤a的20％，a即为碱土离子含量(Ca、Mg、Sr和Ba)的摩尔数。
根据本发明优选实施例，铕掺杂级d2≥a的0.0001％且≤a的2％，a即为碱土离子含量(Ca、Mg、Sr和Ba)的摩尔数。
根据本发明优选实施例，所述至少一种发光材料的发射光谱的半峰全宽(FWHM)为≥120nm。
已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
优选地，所述至少一种发光材料的发射光谱的半宽≥130nm，更优选地≥140nm。
根据本发明优选实施例，所述至少一种发光材料的发射光谱表现出复合发射带，该复合发射带包括：波长范围在≥500nm且≤600nm，优选地≥530nm且≤570nm以及半峰全宽(FWHM)≥80nm，优选地≥100nm且最优选地≥120nm的至少一个最大值；以及波长范围在≥600nm且≤650nm，优选地≥600nm且≤620nm以及半峰全宽(FWHM)≥30nm且≤140nm，优选地≤120nm且最优选地≤100nm的第二个发射最大值。
已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
无需说，该发射光谱可以是这两个发射的叠加(对于本发明这一实施例内的大多数应用而言，实际情况即是如此)，因此可观察到仅仅一个发射最大值。这两个发射随后可以通过去卷积来计算。
根据本发明优选实施例，在使用400nm至480nm光谱范围内的光发射激励之后，该发光材料在500nm至700nm波长间隔内的相对发射能量≥50％，更优选地≥75％。
根据本发明优选实施例，所述至少一种发光材料中的比例[M]∶[Si]，即，(b+y)∶(c+x)，为≥1.01且≤1.20。于此，已经惊奇地发现，对于本发明内的宽范围应用而言，(光)热稳定性甚至可以进一步提高。
优选地，所述至少一种发光材料中的比例[M]∶[Si]为≥1.02且≤1.18，更优选地，所述至少一种发光材料中的比例[M]∶[Si]为≥1.03且≤1.15。
已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
根据本发明优选实施例，(b+y)≥2*d1，更优选地(b+y)≥5*d1。已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
根据本发明优选实施例，在所述至少一种发光材料中，b≥5*y，优选地b≥10*y，更优选b≥20*y。已经表明，对于本发明内的宽范围应用，这可获得对于本发明内的宽范围应用具有进一步改进的照明特征的材料。
根据本发明优选实施例，在所述至少一种发光材料中，c≥10*x，更优选地c≥20*x，更优选c≥50*y。已经表明对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
根据本发明优选实施例，在所述至少一种发光材料中，d1≤0.1。优选地d1≤0.03，更优选d1≤0.01。
根据本发明优选实施例，在所述至少一种发光材料中，[Ba]+[Sr]+[Mg]≤0.9*[Ca]，优选地[Ba]+[Sr]+[Mg]≤0.7*[Ca]且更优选地[Ba]+[Sr]+[Mg]≤0.5*[Ca]。已经表明，对于本发明内的宽范围应用，这可获得具有进一步改进的照明特征的材料。
优选地，该至少一种材料作为粉末提供和/或作为陶瓷材料提供。
如果该至少一种材料至少部分地作为粉末提供，该粉末尤为优选地具有≥2μm且≤15μm的d50。对于本发明内的宽范围应用，已经表明这是有益的。
根据本发明优选实施例，该至少一种材料至少部分地作为至少一种陶瓷材料提供。
在本发明的意义上，措辞“陶瓷材料”特别是指和/或包括具有受控数量的孔隙或者没有孔隙的结晶或多晶的紧凑材料或复合材料。
在本发明的意义上，措辞“多晶材料”特别是指和/或包括体积密度大于主成份的90％的材料，其由大于80％的单晶畴组成，每个畴直径大于0.5μm且具有不同的晶体学取向。单晶畴可以通过无定形或玻璃状材料来连接或者通过另外的结晶成份来连接。
根据本发明优选实施例，提供一种发光装置，特别是LED，其包括平均直径≥100μm至≤2000μm，更优选地≥200μm至≤1500μm，甚至更优选地≥250μm至≤1000μm以及最优选地≥300μm至≤750μm的至少一种陶瓷材料。
根据优选实施例，该至少一种陶瓷材料的体积≥0.005mm3至≤8mm3，更优选地≥0.03mm3至≤1mm3以及最优选地≥0.08mm3至≤0.18mm3。
根据优选实施例，该至少一种陶瓷材料的密度为≥理论密度的90％且≤理论密度的100％。对于本发明内的宽范围应用，已经表明这是有益的，因为这样可以提高至少一种陶瓷材料的发光属性。
更优选地，该至少一种陶瓷材料的密度≥理论密度的97％且≤理论密度的100％，更优选地≥98％且≤100％，再优选地≥98.5％且≤100％以及最优选地≥99.0％且≤100％。
根据本发明优选实施例，该至少一种陶瓷材料的表面的表面粗糙度RMS(表面平坦性的破坏；作为最高和最深表面特征之间的差值的几何平均值来测量)≥0.001μm且该表面粗糙度RMS≤1μm。
根据本发明实施例，该至少一种陶瓷材料的表面的表面粗糙度≥0.005μm且≤0.8μm，根据本发明一实施例，该表面粗糙度≥0.01μm且≤0.5μm，根据本发明一实施例，该表面粗糙度≥0.02μm且≤0.2μm，且根据本发明一实施例，该表面粗糙度≥0.03μm且≤0.15μm。
根据本发明优选实施例，该至少一种陶瓷材料的比表面积≥10-7m2/g且≤0.1m2/g。
根据本发明的材料和/或照明装置可以在各种各样系统和/或应用中使用，包括下述一个或多个系统和/或应用：
-办公室照明系统，
-家庭应用系统，
-商店照明系统，
-家居照明系统，
-重点照明系统，
-聚光照明系统，
-剧院照明系统，
-光纤应用系统，
-投影系统，
-自点亮显示系统，
-像素化显示系统，
-分段显示系统，
-警告标志系统，
-医疗照明应用系统，
-指示标志系统，以及
-装饰照明系统，
-便携式系统，
-车辆应用，
-温室照明系统。
前述组件、以及所主张的组件和在所述实施例中依据本发明将使用的组件在其尺寸、形状、材料选择和技术概念方面没有任何特别例外，使得相关领域中已知的选择标准可以被应用而无限制。
附图说明
本发明目的的附加细节、特征、特性及优点在从属权利要求、附图以及各附图和实例的下述描述中披露，下述描述以示例性方式示出用于本发明照明系统的发光材料的多个实施例和实例以及本发明照明系统的多个实施例和实例。
图1示出本发明的两个照明系统的两个发射光谱，其中在不同蓝色波长发光的LED与本发明实例I的发光材料组合。
图2示出图1的两个照明系统的CIE 1976色坐标，该照明系统具有不同厚度的发光陶瓷板。
图3示出图2在白色区域内的放大图。
图4示出采用了本发明实例I的不同厚度发光陶瓷板的本发明另外照明系统的若干发射光谱。
图5示出采用了本发明实例I的不同厚度发光陶瓷板的本发明另外照明系统的另外若干发射光谱。
图6示出本发明实例I的发光材料的x-y-色点坐标与温度的图示。
具体实施方式
通过下述实例I将进一步理解本发明，实例I仅仅以说明方式示出本发明的若干种材料。
实例I
实例I涉及
1.080(CaN2/3)*1.006(AlN)*0.963(SiN4/3)*0.0198 CeO3/2*0.0002EuO*0.018SiO2*0.014AlO3/2
其按下述方式制备：
所有动作是在干燥惰性气体气氛内进行。53.37克Ca3N2(2N)、41.02克AlN(3N)、0.78克Al2O3、45.30克Si3N4、1.09克SiO2、3.41克CeO2(4N)和0.035克Eu2O3(4N)通过球磨而紧密混合且混合物随后在合成气体气氛(N2∶H295∶5体积/体积)内在1500℃最高温度煅烧。所得到的粉饼再次被研磨、粒化并通过单向加压及随后冷等静压而压制成丸，直至达到＞50％的生坯密度。这些丸在1650℃在合成气体气氛内烧结，可选地随后进行1kbar N2的热等静压步骤以提高密度。
图1示出白色LED发射光谱，该照明系统具有由实例I的材料制成的发光陶瓷板，该发光陶瓷板在主发射波长为450nm的蓝色LED 1以及主发射波长为464nm的蓝色LED 2上的厚度为150μm。两个1mm2薄膜倒装芯片InGaN-GaN LED均通过折射率为1.5的透明胶剂(硅酮)而光学耦合到形成照明系统外表面的发光陶瓷板。除了陶瓷板的光学功能性之外，陶瓷板还形成用于LED的底层粗糙化n-GaN层的刚性机械保护。
可以看出，根据实例I的材料在500nm至700nm波长范围内具有宽带，形成相关色温(CCT)在3000K和4000K之间的照明系统的暖白色发射光谱。
图2示出具有图1的发光陶瓷板的LED(＝照明系统)的色点以及CIE 1976图内使用的蓝色LED的色点。
图3示出图2的白色区域的放大图示。从该图示中看出，该发光材料的特定属性抵消蓝色LED发射的变动。这一属性对于在通用照明应用中白色LED实现稳定白色发射颜色(稳定CCT)是非常有益的，即使LED发射光谱由于驱动电流和结温度变动而变化。
图4和5分别示出具有蓝色泵浦LED的选定白色发光LED的发射光谱，图4为LED 1以及图5为LED 2。
可以示出，使用根据实例I的材料，可以制作具有低CCT和出色显色指数Ra及高显色指数R9的若干LED。R9为饱和红色的再现的度量。数据示于表I和II，其中表I涉及图4的光谱且表II涉及图5的光谱。
表I
  CCT[K]   4411   3583   3323   3286   3256   3231   3210
  Ra   82   76   73   73   73   73   72
  Δuv   0.025   0.006   0.004   0.006   0.007   0.008   0.009
  x   0.3535   0.3942   0.4207   0.4251   0.4289   0.4323   0.4352
  y   0.3116   0.3701   0.4081   0.4144   0.4199   0.4247   0.429
  LE[lm/W]   273   307   327   330   333   335   337
  R1   87.5   76.8   72.2   71.5   70.9   70.4   70
  R2   86.1   81.2   78.1   77.6   77.2   76.9   76.6
  R3   77.6   80.9   81.1   81.2   81.3   81.4   81.5
  R4   81.7   75.5   73.8   73.5   73.3   73.1   73
  R5   85.2   74.2   69.2   68.4   67.8   67.2   66.8
  R6   75.7   70.7   66.6   66.1   65.6   65.1   64.8
  R7   82.9   82.7   83.9   84.2   84.5   84.8   85.1
  R8   81.2   67.9   63   62.3   61.7   61.2   60.8
  R9   55.3   17.7   3.2   1   -0.7   -2.2   -3.5
  R10   60.4   52   46.4   45.6   44.9   44.3   43.8
  R11   78.3   69.8   67.1   66.7   66.3   66   65.7
  R12   63.3   49.9   40.3   38.8   37.6   36.5   35.6
  R13   85.5   76.6   72   71.4   70.8   70.3   69.9
  R14   85.6   88.2   88.6   88.7   88.7   88.8   88.9
表II
  CCT[K]   4587   3597   3395   3274   3230   3194   3163   3138
  Ra   89   81   79   77   76   76   75   75
  Δuv   0.021   0.006   0   0.003   0.005   0.006   0.007   0.008
  x   0.3505   0.3942   0.4109   0.4228   0.4275   0.4316   0.4353   0.4385
  y   0.3167   0.3716   0.3927   0.4076   0.4135   0.4187   0.4233   0.4273
  LE[lm/W]   275   306   317   324   327   330   332   334
  R1   92.1   80.9   77.1   74.6   73.7   72.9   72.2   71.6
  R2   94.8   89.4   85.9   83.6   82.7   81.9   81.3   80.7
  R3   93.2   91.1   89.6   88.5   88.1   87.7   87.4   87.1
  R4   83.1   75.7   73.9   72.8   72.3   72   71.6   71.4
  R5   88.7   78.2   74.1   71.3   70.3   69.4   68.6   67.9
  R6   85.9   80.6   76.5   73.5   72.4   71.4   70.6   69.8
  R7   87.8   86.5   87   87.4   87.6   87.7   87.9   88.1
  R8   84.7   69.5   65.8   63.5   62.6   61.8   61.2   60.7
  R9   69.4   26.7   15.7   8.6   5.9   3.7   1.7   0.1
  R10   87.9   69.6   62.6   57.9   56.2   54.7   53.4   52.3
  R11   75.9   67.7   65.6   64.2   63.7   63.2   62.8   62.5
  R12   65.6   55.8   48.4   42.9   40.7   38.8   37.2   35.6
  R13   94.1   82.9   78.7   76   74.9   74.1   73.3   72.6
  R14   95.9   94.3   93.3   92.7   92.5   92.3   92.1   92
图6示出根据本发明实例I的发光材料的x-y-色坐标(CIE 1931)与温度的图示。图中可以清楚地看出，x-y-色点随温度变化近乎保持恒定，这使得本发明的宽范围的照明系统具有出色的颜色稳定性。
上文详细实施例中的要素和特征的具体组合仅仅是示例性的；这些教导与本发明以及通过引用而结合于此的专利/申请的其他教导的互换和替代也被特别地考虑在内。如本领域技术人员将理解，本领域普通技术人员可以想到此处所述方案的变型、调整和其他实施方式，而不背离所要求保护的本发明的精神和范围。相应地，前述描述仅仅是示例而非限制。本发明的范围在下述权利要求及其等同特征中定义。此外，说明书和权利要求中的参考符号不限制所要求保护的本发明的范围。

Claims (21)

1.一种照明系统，包括成份大致如下的至少一种磷光体材料：
a(AEN2/3)b(MN)c(SiN4/3)d1CeO3/2d2EuO x SiO2y AlO3/2
其中AE为选自Ca、Mg、Sr和Ba或其混合物的碱土金属，且M为选自Al、B、Ga、Sc或其混合物的三价元素，
其中
0.95≤2(a+d1+d2)/(b+c+x+y)≤1.2
a+d1+d2≥c+x，
(b+y)∶(c+x)≥1，
(b+y)≤1+10d1，
b≥5y，
c≥10x，
0.0001≤d1≤0.2且d1≥10d2。
2.如权利要求1所述的照明系统，其中d1≥a的0.01％且≤a的20％。
3.如权利要求1或2所述的照明系统，其中所述至少一种发光材料中(b+y)∶(c+x)的比例≥1.01且≤1.20。
4.如权利要求1或2所述的照明系统，其中在所述至少一种磷光体材料中，(b+y)≤1+10d1。
5.如权利要求1或2所述的照明系统，其中在所述至少一种磷光体材料中，b≥5y且c≥10x。
6.如权利要求1或2所述的照明系统，其中在所述至少一种磷光体材料中，d1≤0.01。
7.如权利要求1或2所述的照明系统，其中所述至少一种发光材料的发射光谱的半峰全宽(FWHM)≥120nm。
8.如权利要求1或2所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥500nm且≤600nm，以及半峰全宽(FWHM)≥80nm的发射最大值。
9.如权利要求8所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥500nm且≤600nm，以及半峰全宽(FWHM)≥100nm的发射最大值。
10.如权利要求9所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥500nm且≤600nm，以及半峰全宽(FWHM)≥120nm的发射最大值。
11.如权利要求8所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥530nm且≤570nm，以及半峰全宽(FWHM)≥80nm的发射最大值。
12.如权利要求11所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥530nm且≤570nm，以及半峰全宽(FWHM)≥100nm的发射最大值。
13.如权利要求12所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥530nm且≤570nm，以及半峰全宽(FWHM)≥120nm的发射最大值。
14.如权利要求1或2所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥600nm且≤650nm，以及半峰全宽(FWHM)≥30nm且≤140nm的发射最大值。
15.如权利要求14所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥600nm且≤650nm，以及半峰全宽(FWHM)≥30nm 且≤120nm的发射最大值。
16.如权利要求15所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥600nm且≤650nm，以及半峰全宽(FWHM)≥30nm且≤100nm的发射最大值。
17.如权利要求14所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥600nm且≤620nm，以及半峰全宽(FWHM)≥30nm且≤140nm的发射最大值。
18.如权利要求17所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥600nm且≤620nm，以及半峰全宽(FWHM)≥30nm且≤120nm的发射最大值。
19.如权利要求18所述的照明系统，其中所述至少一种发光材料的发射光谱表现出复合发射，该复合发射包括：波长范围在≥600nm且≤620nm，以及半峰全宽(FWHM)≥30nm且≤100nm的发射最大值。
20.如权利要求1或2所述的照明系统，其中在所述至少一种发光材料中，[Ba]+[Sr]+[Mg]≤0.9[Ca]。
21.一种包括如权利要求1至20任意一项所述的照明系统的系统，该系统在一个或多个下述应用中使用：
-办公室照明系统，
-家庭应用系统，
-商店照明系统，
-家居照明系统，
-重点照明系统，
-聚光照明系统，
-剧院照明系统，
-光纤应用系统，
-投影系统，
-自点亮显示系统，
-像素化显示系统，
-分段显示系统，
-警告标志系统，
-医疗照明应用系统，
指示标志系统，以及
-装饰照明系统，
-便携式系统，
-车辆应用，
-温室照明系统。
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