CN101883835A - 包含绿色发光SiAlON基材料的发光器件 - Google Patents
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Abstract
本发明涉及包含成分为Sr5-y-z-aMySi23-xAl3+xOx+2aN37-x-2a:Euz:Cez1的绿色发光材料的发光器件,特别是LED。已经发现这种材料在绿色波长范围内具有窄的发射,并具有良好的可制作性和稳定性。
Description
技术领域
本发明涉及发光器件领域,具体地涉及LED领域。
背景技术
包括硅酸盐、磷酸盐(例如,磷灰石)以及铝酸盐作为主材料,过渡金属或稀土金属添加到宿主材料作为活化材料的磷光体是广为人知的。特别地,由于蓝色LED近年来已经变得实用,使用这种蓝色LED与这种磷光体材料相组合的白色光源的发展正被积极推行。
特别是基于所谓“SiAlON”系统的发光材料,由于其良好的光学特征,已经成为在该领域关注的焦点。
然而,仍然持续需要这样的发光材料,其在宽范围应用中可使用并特别允许制造具有优化的发光效率和显色的磷光体暖白色pcLED。
特别是在绿色发光磷光体领域中,已经研究了若干种材料。
例如在US 7061024B2中,建议一种成分为SrSi2O2N2:Eu的材料,其容易生产并具有可调谐色点。然而,这种复合物经常缺少色点饱和并对于一些应用具有太宽的光谱。
另一种复合物(Ba,Sr)2SiO4:Eu在US 6555958B1中提到。这里的优点也是良好的可制作性和色点的可调谐性。然而,此处光谱对于很多应用太宽,且已经显示出这种复合物在潮湿空气中具有一些退化趋势。
发明内容
本发明的目的是提供具有一种材料的发光器件,该材料具有改善的光学特性且具有良好的可制作性和稳定性。
由根据本发明权利要求1的发光器件来达成该目的。相应地,包含基本上成分为Sr5-y-z-aMySi23-xAl3+xOx+2aN37-x-2a:Euz:Cez1的绿色发光材料的发光器件,特别是LED,
其中M选自包含Ca、Ba、Mg或其混合物的群组,
且x为≥0到≤7,y为≥0到≤5,a为≥0到≤1.5,z为≥0.0001到≤0.5以及z1为≥0到≤0.5。
措辞“绿色发光”特别是指和/或包括材料在可见光范围内(在受到合适的激发时)显示具有最大值在500nm和600nm之间的发射。
措辞“基本上”特别是指≥95%,优选地≥97%,以及最优选地≥99%的该材料具有所期望的成分。
对于本发明内的宽范围应用,这种材料已经示出具有至少一个下述优点:
-与现有技术的材料比较,该材料的稳定性通常得到改进。该材料通常具有非常高的热稳定性,特别是光热稳定性。
-这种材料的光谱通常相当尖锐,因此允许使用在本发明内的许多应用中。
-该光谱可以被“调谐”(将在稍后描述)。
应该注意到,Ce(III)也可以存在于本发明的材料中。然而,由于Ce(III)通常并入Eu(II)或其它二价离子的位置,附加的正电荷必须通过与纯材料的化学配比的偏离来补偿。这里几种选项是可用的,其对于本领域的技术人员都是已知的:
1.阳离子空位
2.改变SiAlON相中的O/N比例
3.改变Si/Al比例
4.用单价阳离子(例如Na)共掺杂。
根据由于Ce(III)并入而引起改变的材料偏离因此将被本领域技术人员注意到,并也落到上面给出的分子式内。
根据本发明一实施例,y为≥0.5到≤3。已经示出,通过如此,对于许多应用,光谱的“调谐”是可能的。例如用Ca代替一部分Sr导致发射的红移,而用Ba代替一部分Sr导致发射的蓝移。
此外,在本申请内的许多应用中已经发现,降低碱土阳离子浓度(增大因子a)或增加(Si,N)→(Al,O)替换比例(增大因子x)也导致发射带的蓝移,因此此处进一步的“调谐”选项是可能的。
在此上下文中,根据一优选实施例,a被设置为0≤a<1。
根据另一个优选实施例,x被设置为1≤x<4,更优选地X被设置为1.5≤x<3。
根据本发明一优选实施例,绿色发光材料具有正交晶体结构。对于本发明内的许多应用已经发现,通过如此,材料的属性(特别是发射剖面(emission profile))可进一步增强。
根据本发明一优选实施例,在绿色发光材料的晶体结构中Eu(II)和/或Ce(III)被定位在6或7重配位层中。不受任何理论约束,发明人认为通过这种方式设置材料,材料的发射带可以变窄用于许多应用。
根据本发明一优选实施例,在可见光范围内的发射带的半宽为≤90nm。
根据本发明另一实施例,该材料作为陶瓷材料被提供。
措辞“陶瓷材料”从本发明的意义上说特别是指和/或包括结晶或多晶紧凑材料或具有受控数量的孔或没有任何孔的复合材料。
措辞“多晶材料”从本发明的意义上说特别是指和/或包括体积密度大于主要组成的百分之90的材料,该主要组成由大于百分之80的单晶畴构成,每个畴直径大于0.5μm并可能具有不同的晶体学取向。单晶畴可以通过无定形或玻璃态材料或者通过附加的结晶组成来连接。
根据本发明一优选实施例,在以10W/cm2的光功率密度以及2.75eV的平均光子能量在200℃曝光陶瓷材料1000小时之后,陶瓷材料的光热稳定性为≥80%至≤100%。
措辞“光热稳定性”从本发明的意义上说特别是指和/或包括在同时施加热和高强度激发下的发光强度守恒,即100%的光热稳定性表明该材料几乎不受同时辐射和加热的影响。
根据本发明一优选实施例,在以10W/cm2的光功率密度以及2.75eV的平均光子能量在200℃曝光陶瓷材料1000小时之后,陶瓷材料的光热稳定性为≥82.5%到≤95%,优选地为≥85%到≤97%。
根据本发明一优选实施例,陶瓷材料的热导率为≥0.04W cm-1K-1到≤0.15W cm-1K-1。
根据本发明一个实施例,陶瓷材料示出对于从≥550nm到≤1000nm波长范围内的光在空气中垂直入射时的透明度为≥10%到≤85%。
优选地,对于从≥550nm到≤1000nm波长范围内的光,在空气中垂直入射的透明度为≥20%到≤80%,对于从≥550nm到≤1000nm波长范围内的光,更优选地为≥30%到≤75%以及最优选地为>40%到<70%。
措辞“透明度”从本发明的意义上说特别是指不能被该材料吸收的某一波长入射光的≥10%,优选地≥20%,更优选地≥30%,最优选地≥40%且≤85%,对于在空气中垂直入射(以任意角度)而言,透射穿过该样品。该波长优选地在≥550nm且≤1000nm的范围内。
根据本发明一优选实施例,陶瓷材料具有为理论密度的≥95%且≤101%的密度。
根据本发明一优选实施例,陶瓷材料具有为理论密度的≥97%且≤100%的密度。
根据本发明所描述优选实施例的低于100%的密度优选地通过将陶瓷烧结到孔仍存在于陶瓷基体中的阶段来获得。最优选地是,密度在≥98.0%且≤99.8%的范围内,陶瓷基体中总的孔体积在≥0.2%至≤2%的范围内。优选的平均孔径在≥400nm至≤1500nm的范围内。
根据本发明的发光器件以及使用本方法生产的陶瓷材料可以用于各种各样的系统和/或应用中,以下的一种或多种在这些系统和/或应用之中:
-办公室照明系统,
-家庭应用系统,
-商店照明系统,
-居家照明系统,
-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,
-指示器标志系统,以及
-装饰照明系统,
-便携式系统,
-汽车应用,
-温室照明系统。
前面提到的部件、以及要求保护的部件和在所述实施例中根据本发明使用的部件,就它们的尺寸、形状、材料选择和技术构思而言不存在任何特殊例外,使得相关领域中已知的选择标准可以不受限制地被应用。
附图说明
在从属权利要求、图和对各图及实例的以下描述中披露了本发明目的的附加细节、特征、特性和优势,其中各图及实例以示例性方式示出在根据本发明的发光器件中使用的材料的若干实施例和实例。
图1示出根据本发明实例I的材料的XRD图案。
图2示出根据实例I的材料的发射和激发光谱。
图3示出描述本发明实例I的材料的晶体结构的第一方面的图片。
图4示出描述本发明实例I的材料的晶体结构的第二方面的图片。
图5示出表示实例I的材料中发光离子的配位点的图片。
图6示出实例I的材料的宏观结构的照片。
具体实施方式
实例I
连同实例I将更好地理解本发明,其中实例I以纯粹说明性方式地作为本发明的绿色发光材料的一个实例。
实例I涉及Sr4.9Al5Si21O2N35:Eu0.1,其以如下方式制作:16.4克AlN(98.5%)、35.14克SrH2(98.5%)、1.41克Eu2O3(99.99%)和82.3克SiNxOy(x=1.66,y=0.02)在惰性气氛下在塑料盒中混合,并在1550℃煅烧(firing)两次,两次煅烧之间具有中间研磨。
得到的粉末用水清洗并干燥。
图1示出由于晶体内堆叠无序而包含尖锐和漫反射的SiAlON磷光体的XRD图案。无序程度可受煅烧温度分布图的停留时间和冷却速率影响。令人惊讶地发现,层堆叠的高度无序不影响发光材料的效率。尖锐的反射(由红线表示)可以用具有 以及的正交子晶胞标记。包含漫反射的完整图案用M5Si23-xAl3+xOxN37-x结构沿c方向的八重拉长晶胞来描述。
图2示出实例I的材料的发射(EM,450nm激发)和激发(EXC,在525nm处监测)光谱。发现磷光体的CIE色点为:x=0.27,y=0.63。因而,单独这种材料对于绿色发光应用非常有用;然而,采用例如(Ba,Sr,Ca)2Si5-xAlxN8-xOx:Eu,(Sr,Ca,Ba)Al1+xSi4-xN7-xOx:Eu或(Ca,Sr,Mg)Si1-xAl1+xN3-xOx:Eu,Ce的另外红色发光磷光体,可以提供白色光用于许多应用。
为了理解本发明的发明属性,实例I的材料的晶体结构使用图3至5进一步解释,这些图示出所确定的结构的几种详细示图。
从图3可以看到,该材料结晶呈复杂结构,其由以Si为主中心阳离子的角连接的(Si,Al)(O,N)4四面体的起伏层和以Al为主中心阳离子的角和边连接的(Si,Al)(O,N)4四面体的更为平坦层的堆叠构建而成。图2示出角和边连接的(Si,Al)(O,N)4四面体的平坦层的一部分。共享边的四面体优选地被Al原子占据,然而如果电荷补偿通过调整N/O比例正确地进行,Si原子也可以被构建在内。
在图中,Al(N,O)4四面体用指数I标记,Si(N,O)4四面体用指数II标记。“Sr位”(其也被Eu占据)用指数III标记。
该结构的单位晶胞用指数IV标记。在一个分子式单位中存在30个只能由N原子占据的3重连接阴离子位,以及7个可由N和O二者占据的2重连接阴离子位。
从图4可以看到,该结构包含边和旋涡连接的四面体的层。发现共享边的四面体位通常被Al占据,尽管这不是“必须的”。
图5示出存在于本发明材料的结构中的三个晶体学上独立的阳离子位的坐标(其标记为Sr1、Sr2、Sr3,不过Eu当然也将占据这些位)。所有位示出类似的具有6或7重坐标的配位层(接触短于),这(尽管不受这个解释的约束)可帮助解释Eu(II)掺杂的磷光体材料的相当狭窄的发射带。
图6示出实例I材料的宏观结构的照片。令人惊讶地,材料自发地生长在相当大的板状微晶中。
实例I的材料特征特别地用于生产具有高光学质量的陶瓷。
上面详细描述实施例中的要素和特征的具体组合仅仅是示范性的;这些教导与此申请以及通过引用而并入的专利/申请中的其它教导的互换和替代也被清楚地考虑到。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、修改和其它实施方式,而不背离所要求保护的本发明的精神和范围。相应地,前述描述仅仅是通过示例的方式,而意图是非限制性的。本发明的范围在下述权利要求书及其等效描述中限定。此外,说明书和权利要求书中使用的附图标记不限制所要求保护的本发明范围。
Claims (10)
1.包含基本上成分为Sr5-y-z-aMySi23-xAl3+xOx+2aN37-x-2a:Euz:Cez1的绿色发光材料的发光器件,特别是LED,
其中M选自包含Ca、Ba、Mg或其混合物的群组,
且x为≥0到≤7,y为≥0到≤5,a为≥0到≤1.5,z为≥0.0001到≤0.5以及z1为≥0到≤0.5
2.如权利要求1所述的发光器件,其中y为≥0.5到≤3。
3.如权利要求1或2所述的发光器件,其中a为≥0到≤1。
4.如权利要求1至3中任意一项所述的发光器件,其中x为≥1到≤4。
5.如权利要求1至4中任意一项所述的发光器件,其中该绿色发光材料具有正交晶体结构。
6.如权利要求1至5中任意一项所述的发光器件,其中在该绿色发光材料的晶体结构中Eu(II)和/或Ce(III)被定位在6或7重配位层中。
7.如权利要求1至6中任意一项所述的发光器件,其中该材料在可见光范围内的发射带的半宽为≤90nm。
8.如权利要求1至7中任意一项所述的发光器件,其中该材料作为陶瓷材料被提供。
9.如权利要求1至8中任意一项所述的发光器件,其中该陶瓷材料用10W/cm2的光功率密度以及2.75eV的平均光子能量在200℃曝光1000小时之后,该陶瓷材料的光热稳定性为≥80%到≤100%。
10.包含如权利要求1至9中任意一项所述的发光器件的系统,该系统用于一种或多种下述应用:
-办公室照明系统,
-家庭应用系统,
-商店照明系统,
-居家照明系统,
-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,
-指示器标志系统,以及
-装饰照明系统,
-便携式系统,
-汽车应用,
-温室照明系统。
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