CN101883834B - 具有减少的散射的用于led的陶瓷材料及其制作方法 - Google Patents

具有减少的散射的用于led的陶瓷材料及其制作方法 Download PDF

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CN101883834B
CN101883834B CN200880118932.9A CN200880118932A CN101883834B CN 101883834 B CN101883834 B CN 101883834B CN 200880118932 A CN200880118932 A CN 200880118932A CN 101883834 B CN101883834 B CN 101883834B
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ceramic transducer
present
lighting systems
transducer material
ceramic
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CN101883834A (zh
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A·蒂克斯
P·J·施密特
H-H·贝希特尔
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Koninklijke Philips NV
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Abstract

本发明涉及一种通过单轴热压步骤来制作的具有减少的散射的用于LED的陶瓷发光材料。

Description

具有减少的散射的用于LED的陶瓷材料及其制作方法
技术领域
本发明涉及用于发光器件、具体为用于LED的发光材料。
背景技术
包括硅酸盐、磷酸盐(例如，磷灰石)和铝酸盐作为宿主材料的荧光体众所周知，其中过渡金属或者稀土金属作为激活材料添加到宿主材料。具体而言，由于蓝色LED近年来已经变得实用，所以正在踊跃地追求将这样的蓝色LED与这样的荧光体材料结合用来开发白光源。随着陶瓷发光材料的问世，蓝色LED也可以几乎完全转换成绿色或者红色。
具体而言，基于所谓“SiAlON”系统的发光材料由于它们的良好光学特征而在业内成为关注焦点。
然而，仍然持续需要如下发光材料，这些发光材料可用于广泛应用中并且尤其允许制造发光效率和显色性优化的荧光体暖白色pcLED。
发明内容
本发明的目的在于提供一种光学特征改进而具有良好的可生产性和稳定性的包括发光材料的发光器件。
这一目的通过根据本发明的权利要求1的一种发光器件来实现。因而，提供一种发光器件、具体为LED，该发光器件包括发射第一波长的至少一种第一发光材料和至少一种陶瓷转换器材料，该陶瓷转换器材料至少部分地吸收第一波长并且随后发射比第一波长更大的第二波长的光，所述陶瓷转换器材料具有在20°的散射强度SI(20)和在40°的散射强度SI(40)，其中SI(20)/SI(40)＞1.5。
术语“在Y°的散射强度SI(Y)”定义如下：
将100μm晶片抛光至光学质量(Ra＜20nm)。在陶瓷转换器材料上的法线入射(＝垂直于晶片)之下发射波长为λ的单色光，其中在吸收系数a＜30cm-1的可见光谱区中选择λ。
在0°角(＝垂直于晶片)测量的散射强度(＝在散射角的透射光)为100％(也参见图3)。然后在Y°角测量在Y°的散射强度SI(Y)。
术语“陶瓷转换器材料”就本发明而言具体意味着和/或包括孔数量受控制或者无孔的晶体或者多晶密实材料或者复合材料。
术语“多晶材料”就本发明而言具体意味着和/或包括如下材料，该材料的体积密度大于主要组成的百分之九十，该主要组成包括多于百分之八十的单晶域，各域的直径大于0.5μm，并且该材料可以具有不同结晶定向。单晶域可以由非晶形材料或者玻璃状材料或者由附加结晶组成来连接。
已经发现根据本发明的陶瓷转换器材料对于许多应用而言具有以下优点中的至少一个或者多个优点：
-发现的光学散射增强器件的转换效率，因为散射可能导致吸收损耗。
-发现的光学散射增强转换光与透射的非转换光的混合并且提供高封装效率。
优选地，陶瓷转换器材料具有在20°的散射强度SI(20)和在40°的散射强度SI(40)，其中SI(20)/SI(40)＞1.6，优选地SI(20)/SI(40)＞1.8。
根据本发明的一个优选实施例，陶瓷转换器材料具有在30°的散射强度SI(30)和在60°的散射强度SI(60)，其中SI(30)/SI(60)＞1.9。这针对本发明内的许多应用进一步增加转换效率。
优选地，陶瓷转换器材料具有散射强度比SI(30)/SI(60)＞2.5，优选为SI(30)/SI(60)＞2.9。
根据本发明的一个优选实施例，陶瓷转换器材料表明它的组成微晶颗粒的优选定向，该定向定义为它的纹理。
为了检测优先定向，可以应用X射线衍射技术。无优先定向的陶瓷展现如下X射线衍射图案，这些图案的相对峰值强度与针对对应材料计算的相对峰值强度相同。对X射线图案的计算需要知道材料的晶体结构，但是关于晶体形态的信息并非必需。纹理化陶瓷的X射线衍射图案表明峰值强度与理论图案相比的显著偏离，即一些反射表明增强的强度而其他反射可能展现甚至降至检测限以下的强度。由其Miller指标表征的哪些反射表明增加或者减少的强度一般依赖于测量几何形状(即陶瓷样本相对于X射线束的对准)、样本内的颗粒形态以及定向。
优选地，陶瓷转换器材料表明它的组成微晶颗粒的优选定向，从而Int峰值A∶Int峰值B≥3、优选为≥5、更优选为≥7并且最优选为≥9，其中Int峰值A∶Int峰值B定义如下：
对于与宿主化合物SrSi2O2N2同型的一般组成为Sr1-x-yMxEuySi2O2N2的化合物，其中M＝Ca、Ba、Mg或者其混合物，Int峰值A由(020)反射的强度(以(0k0)晶格平面平行于晶体结构中的[Si2O2N2]2-层这样的方式选择结晶设置)或者由(020)和(120)反射的强度之和(如果峰值在XRD粉末图案中未充分地分离以确定(020)反射的强度)给定，而Int峰值B由(220)反射的强度或者由(220)和(2-10)反射的强度之和(如果峰值在XRD粉末图案中未充分地分离以确定(220)反射的强度)给定。
根据本发明的一个优选实施例，陶瓷转换器材料实质上由d50≥5μm的颗粒制成。已经表明这在广泛应用中进一步减少散射。
术语“实质上”在本发明的背景中具体意味着材料的≥75％、优选为≥80％并且最优选为≥90％具有所需组成和/或结构。
术语“d50”就本发明而言为针对平均粒子尺寸的测量并且定义如下：对应样本中的粒子(例如颗粒)的数目的50％的尺寸等于或者小于给定d50值。术语“粒子尺寸”具体代表其体积与具有任意形状的所考虑的粒子的体积相等的球体的直径。
优选地，陶瓷转换器材料实质上由d50≥7μm的颗粒制成。
根据本发明的一个优选实施例，该材料实质上具有以下组成：
Sr1-y-zMySi2O2N2:Euz
其中M选自于包括Ca、Ba、Mg或者其混合物的组，
并且y≥0至≤1，而z≥0.0001至≤0.5。
这样的材料已经表明由于以下原因而有利于广泛应用：
-材料的稳定性与现有技术的材料相比通常有所改进。材料通常具有很高的热稳定性、尤其是光热稳定性。
-该材料的光谱通常相当锐利，因此允许使用于本发明内的许多应用。
根据本发明的一个优选实施例，在200℃、光功率强度为10W/cm2而平均光子能量为2.75eV时将陶瓷转换器材料曝光1000小时之后，陶瓷转换器材料的光热稳定性为初始强度的≥80％至≤110％。
术语“光热稳定性”就本发明而言具体意味着和/或包括在同时施加热和高强度激发之下发光强度的保持，即100％的光热稳定性表明材料实际上不受同时暴露于辐射和热所影响。
根据本发明的一个优选实施例，在200℃、光功率强度为10W/cm2而平均光子能量为2.75eV时将陶瓷转换器材料曝光1000小时之后，陶瓷转换器材料的光热稳定性为≥82.5％至≤105％、优选为≥85％至≤100％。
根据本发明的一个优选实施例，陶瓷转换器材料的导热率为≥1W m-1K-1至≤20W m-1K-1。
根据本发明的一个实施例，陶瓷转换器材料表明对于波长范围从≥550nm至≤1000nm的光在空气中法线入射时为≥10％至≤85％的透明度。
优选地，在空气中法线入射时的透明度对于波长范围从≥550nm至≤1000nm的光为≥20％至≤80％、更优选为≥30％至≤75％并且对于波长范围从≥550nm至≤1000nm的光最优选为＞40％至＜70％。
术语“透明度”就本发明而言具体意味着：
在空气中法线入射(＝垂直于表面)时经过样本透射波长不为材料所吸收的入射光的≥10％、优选为≥20％、更优选为≥30％、最优选为≥40％且≤85％。该波长的范围优选为≥550nm和≤1000nm。
根据本发明的一个优选实施例，陶瓷转换器材料的密度为理论密度的≥95％且≤101％。
根据本发明的一个优选实施例，陶瓷转换器材料的密度为理论密度的≥97％且≤100％。
优选地通过将陶瓷烧结至孔仍然存在于陶瓷基质中的阶段来获得根据本发明上述优选实施例的低于100％的密度。更优选范围为≥98.0％且≤99.8％的密度而陶瓷基质中的总孔体积范围为≥0.2-≤2％。优选平均孔直径范围为≥1000-≤5000nm。
本发明还涉及一种生产本发明材料的方法，该方法包括单轴地热压至少一种前体化合物，该按压步骤在≥1200℃至≤1800℃的温度进行。
已经出乎意料地表明：通过这样做，可以针对许多应用而容易地和高效地生产具有合乎需要和具创造性的特征的材料。
优选地，按压步骤在≥1300℃至≤1700℃的温度进行。
已经出乎意料地发现：对于在本发明内的许多应用，可以通过单轴热压引起多晶陶瓷转换器材料的纹理。在单轴热压期间，板状陶瓷颗粒优先地定向成它们的表面法线在单轴热压方向上。
根据本发明的一个优选实施例，至少一种前体化合物实质上包括纵横比为≥2∶1的晶体颗粒。
术语“纵横比”具体意味着粒子颗粒的最长与最短尺度之比。发现例如板状和针状粒子有大的纵横比。
对于本发明内的许多应用已经表明：通过如上文所言那样做，可以进一步增强通过本发明方法制作的陶瓷转换器材料的所需特征，尤其可以减少光返回入射方向的散射。
优选地，至少一种前体化合物实质上具有≥3∶1、更优选为≥4∶1的纵横比。
根据本发明的一个优选实施例，至少一种前体化合物实质上由直径≥500nm的板和/或片制成。
对于许多应用已经表明这也有助于制造工艺并且降低生产的陶瓷转换器材料的散射。
优选地，至少一种前体化合物实质上由直径≥700nm、更优选为≥1μm的板和/或片制成。
根据本发明的一个优选实施例，在≥50MPa的压强进行按压步骤。
包括根据本发明的陶瓷转换器材料的发光器件以及如利用本发明方法生产的陶瓷转换器材料可以使用于广泛各种系统和/或应用中，这些系统和/或应用比如为以下各项中的一项或者多项：
-办公照明系统
-家用应用系统
-商店照明系统，
-家庭照明系统，
-重点照明系统，
-部位照明系统，
-剧院照明系统，
-光纤应用系统，
-投影系统，
-自照亮显示系统，
-像素化显示系统，
-分段显示系统，
-警告标记系统，
-医疗照明应用系统，
-指示符标记系统，以及
-装饰照明系统
-便携系统
-汽车应用
-温室照明系统。
在描述的实施例中的前述组成以及要求保护的组成和将根据本发明来使用的组成就它们的尺寸、形状、材料选择和技术概念而言无任何特例，从而可以无限制地应用相关领域中已知的选择标准。
附图说明
在从属权利要求、附图以及对相应附图和例子的下文描述中公开了本发明的目的的附加细节、特征、特性和优点，这些附图和例子以举例方式示出了根据本发明的用于在发光器件中使用的材料的若干实施例和例子。
图1示出了根据本发明的例子I的用于材料的XRD图案，
图2示出了根据比较例子I的用于材料的XRD图案，
图3示出了本发明例子I和比较例子I的散射强度的角度分辨测量，
图4示出了本发明例子I和比较例子I的发射光谱，
图5示出了在研磨和抛光之后根据例子I的陶瓷转换器材料的结构的光学显微图，以及
图6示出了用于测量陶瓷转换器材料的纹理的颇具示意性的试验设置。
具体实施方式
根据对例子I的下文具体描述将更好地理解本发明，该例子以仅为示例的方式作为本发明的陶瓷转换器材料的一个例子。本发明例子I和比较例子I均涉及SrSi2O2N2:Eu陶瓷。
例子I
通过碾磨混合掺杂Eu的正硅酸锶(Sr0.98Eu0.02)2SiO4与氮化硅、在N2/H2气氛中在1400℃燃烧混合物并且最终碾磨和筛选原产品来合成公称组成为Sr0.98Eu0.02Si2O2N2的前体粉末。
在石墨按压工具中填充约4克前体粉末、预硬化该粉末并且最终在氮范围中在1500℃和70Mpa将该粉末单轴地热压5小时。
将所得陶瓷体切片、研磨和抛光至100μm的最终厚度。
比较例子I(常规烧结)
通过在惰性气体气氛中碾磨混合掺杂Eu的正硅酸锶(Sr0.98Eu0.02)2SiO4与氮化硅、在N2/H2气氛中在1200℃燃烧混合物并且最终碾磨和筛选原产品来合成公称组成为Sr0.98Eu0.02Si2O2N2的前体粉末。
单轴和均衡地冷压粉末，并且在氮气氛中在环境压力下在1550℃将所得盘形小球烧结5小时。
将所得陶瓷体研磨和抛光至100μm的最终厚度。
图1和图2分别示出了本发明例子I和比较例子I的XRD图案。针对θ＝0°用与板法线垂直定位的入射X射线束获得XRD图案，其中板法线(a)平行于例子I的单轴热压方向和(b)平行于比较例子I的单轴冷压方向。
图3示出了根据本发明例子I(实线)和比较例子I(虚线)、针对100μm厚度的晶片、针对法线入射660nm激光束的透射光的正规化角度散射强度分布。将晶片的表面抛光至光学质量(Ra＜20nm)。光散射因此归因于仅在晶片内的散射事件。
清楚可见本发明的材料的散射明显不同于比较例子的材料的散射。也就是说，在20°的散射强度SI(20)＞在40°的散射强度SI(40)的2倍，而在30°的散射强度SI(30)＞在60°的散射强度SI(60)的3倍，而在比较例子中，这些比值小得多。
图4示出了本发明例子I(实线)和比较例子I(虚线)的蓝色LED上的发射光谱。由于优良的散射特征，本发明例子的发射度特性优于比较例子的发射度特性。
图5示出了在研磨和抛光之后根据例子I的陶瓷转换器材料的结构的光学显微图。可见陶瓷转换器材料包括其中一些直径为50μm或者更多的许多大颗粒和/或板。平均d50约为4μm。不限于任何理论，发明人认为该非正统结构至少部分地造成本发明的材料的具创造性和合乎需要的优点。
下文讨论根据例子I的材料的结构以及根据本发明优选应用的用于测量材料纹理的主要设置。
可以借助X射线衍射来量化陶瓷转换器材料以内的组成微晶颗粒的优选定向。
图6示出了用于测量陶瓷转换器材料的纹理的颇具示意性的试验设置。在陶瓷样本3中，表明两个板状陶瓷微晶1和2，这些微晶的晶格平面几乎垂直于或者——如针对高度纹理化的陶瓷所希望的那样——垂直于板法线。待考察的陶瓷板3受到入射X射线束6。用X射线检测器7测量衍射光束5。θ为衍射角。陶瓷板的表面法线与箭头4所示的在单轴热压期间的按压方向重合。
可以如在通过引用完全结合于此的非专利文献M.D.Vaudin等人的J.Mater.Res.13(1998)2910中所述，通过组合越过优选定向反射峰值的θ-2θ扫描与θ扫描来完成结晶纹理的量化确定。
如果以针对θ＝0°将入射X射线束与陶瓷的单轴热压方向垂直定位这样的方式进行X射线衍射试验，则针对与按压方向垂直的板状微晶颗粒的倒易晶格平面优先地观测造成X射线辐射衍射最大值的结构干涉。如果以针对θ＝90°将检测器与正交于陶瓷样本的平面平行定位这样的方式进行Bragg-Brentano几何结构中的X射线检测器的对称θ-2θ扫描，则极大增强如下反射，这些反射源于在与按压方向垂直或者接近垂直定向的晶格平面处的衍射，而极大削弱如下反射，这些反射源于在与按压方向平行或者接近平行定向的晶格平面处的衍射。
对例子I的材料的进一步考察给出以下结果。
根据例如在通过引用全部结合于此的O.Oeckler、F.Stadler、T.Rosenthal、W.Schnick的Solid State Sci.，2009，9(2)，205-212中描述的晶体结构确定结果，由拐角共享[SiON3]四面体的片以及形成Sr或者掺杂物离子(这些离子位于[Si2O2N2]片之间)的配位环境的末端氧离子来形成SrSi2O2N2。因此，可以针对SrSi2O2N2前体化合物观测板状形态。
对于包括板状颗粒的热压SrSi2O2N2:Eu型陶瓷，在例子章节中说明了细节。在以下章节中说明一种用于盘形陶瓷样本的一般适用测量几何结构(如在下述所有测量中应用的那样)。
关于该结构，(0k0)倒易晶格平面与[Si2O2N2]片平行定向、因此也正交于SrSi2O2N2板法线。对于具有显著优先定向的样本，尤其是具有Miller指数(0k0)的反射表明与其他反射相比增加的强度。在2θ～12.6°发现SrSi2O2N2的(010)反射，而(020)峰值在2θ～25.4°与(120)峰值重叠(两个峰值之和将称为峰值A)。在2θ～31.8°发现具有最大理论强度即(220)峰值的反射，并且该反射与(2-10)反射重叠(两个峰值之和将称为峰值B)。
比较热压(本发明例子I)和常规烧结(比较例子I)的材料的XRD图案，变得清楚的是热压获得如下陶瓷，这些陶瓷具有微晶的强优先定向。即使在2θ～12.6°的峰值仍然表明比峰值B更高的强度。
根据比较例子I的陶瓷未展现显著优先定向并且表明强度比Int峰值A∶Int峰值B＜1(也参见图7)，而Int峰值A∶Int峰值B＞1表明优先定向的存在。
具有强优先定向的样本应当展现Int峰值A∶Int峰值B＞3、优选为＞5的比值。对于上述热压陶瓷(本发明例子I)，观测到Int峰值A∶Int峰值 B～9.4的强度比(基于本底校正后的峰值高度)，这表明可以观测到很强优先定向。
在上文详述的实施例中的单元和特征的特定组合仅为举例；也明确构思这些教导与在本专利和引用结合的专利/申请中的其他教导的互换和替换。如本领域技术人员将认识到的那样，本领域普通技术人员可以想到对这里所述内容的变化、修改和其他实施而不脱离如要求保护的本发明的精神和范围。因而，前文描述仅为举例而非作为限制。在所附权利要求及其等效内容中限定本发明的范围。另外，在说明书和权利要求书中使用的参考标号并不限制如要求保护的本发明的范围。

Claims (9)

1.一种用于发光器件、具体为LED的陶瓷转换器材料，具有在20°的散射强度SI(20)和在40°的散射强度SI(40)，其中SI(20)/SI(40)＞1.6，
其中所述材料实质上具有如下组成：
Sr1-y-zMySi2O2N2:Euz
其中M选自于包括Ca、Ba、Mg或者其混合物的组，
并且y≥0至≤1，而z≥0.0001至≤0.5。
2.根据权利要求1所述的陶瓷转换器材料，具有在30°的散射强度SI(30)和在60°的散射强度SI(60)，其中SI(30)/SI(60)＞1.9。
3.根据权利要求1或者2所述的陶瓷转换器材料，其中所述陶瓷转换器材料表明它的组成微晶颗粒的优选定向。
4.根据权利要求1或2所述的陶瓷转换器材料，其中所述材料实质上由d50≥5μm的颗粒制成。
5.一种生产根据权利要求1至4中的任一权利要求所述的材料的方法，包括单轴地热压至少一种前体化合物，所述按压步骤在≥1200℃至≤1800℃的温度进行。
6.根据权利要求5所述的方法，其中所述至少一种前体化合物实质上具有≥2∶1的纵横比。
7.根据权利要求5或者6所述的方法，其中所述至少一个前体化合物实质上由直径≥500nm的板和/或片制成。
8.根据权利要求5或6所述的方法，其中在≥50MPa的压强进行所述按压步骤。
9.一种系统，包括根据权利要求1至4中的任一权利要求所述的材料和/或根据权利要求5至8中的任一权利要求生产的材料，所述系统使用于以下应用中的一个或者多个应用：
-办公照明系统
-家用应用系统
-商店照明系统，
-家庭照明系统，
-重点照明系统，
-部位照明系统，
-剧院照明系统，
-光纤应用系统，
-投影系统，
-自照亮显示系统，
-像素化显示系统，
-分段显示系统，
-警告标记系统，
-医疗照明应用系统，
-指示符标记系统，以及
-装饰照明系统
-便携系统
-汽车应用
-温室照明系统。
CN200880118932.9A 2007-12-03 2008-11-25 具有减少的散射的用于led的陶瓷材料及其制作方法 Active CN101883834B (zh)

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