CN101821357A - 包括多相SiAlON基陶瓷材料的发光器件 - Google Patents

包括多相SiAlON基陶瓷材料的发光器件 Download PDF

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CN101821357A
CN101821357A CN200880111540A CN200880111540A CN101821357A CN 101821357 A CN101821357 A CN 101821357A CN 200880111540 A CN200880111540 A CN 200880111540A CN 200880111540 A CN200880111540 A CN 200880111540A CN 101821357 A CN101821357 A CN 101821357A
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luminescent device
phase
present
described luminescent
ceramic
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CN101821357B (zh
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P·J·斯米特
B·-S·施雷恩马彻尔
A·图克斯
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Koninklijke Philips NV
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Abstract

本发明涉及一种发光器件，包括光源，特别是LED，以及发光材料，该发光材料为基本上具有成分M2-zCezSi5-x-y-(z-z1)Ay+(z-z1)N8-4x-y+z1O4x+y-z1的陶瓷多相材料。该材料已被发现具有至少两相的成分，这导致更好的可制作性以及光稳定性和转换效率。

Description

包括多相SiAlON基陶瓷材料的发光器件
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
磷光体材料(或磷光体)用作波长转换器(或磷光体转换器＝pc)，该波长转换器吸收从光源发射的第一波长并重新发射比第一波长(发光材料)长的第二波长。包括硅酸盐、磷酸盐(例如，磷灰石)以及铝酸盐作为宿主材料、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。具体地，由于蓝色LED光源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开发正被积极推进。
特别地基于所谓“SiAlON”系统的发光材料，由于其良好的光学特性，已经成为在该领域中关注的焦点。
然而，仍然持续需要这样的发光材料，其可以在宽范围的应用中使用并特别使得可制造具有优化的发光效率和显色的磷光体暖白色pcLED。
发明内容
本发明的目的是提供一种具有发光材料的发光器件，其具有改善的光学特性且具有良好的可制作性。
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，一种发光器件包括光源，特别是LED，以及发光材料，该发光材料为基本上具有下述成分的陶瓷多相材料：
M2-zCezSi5-x-y-(z-z1)Ay+(z-z1)N8-4x-y+z1O4x+y-z1
其中M选自包括Sr、Ca、Ba、Mg、Eu或其混合物的群组，
A选自包括Al、B、Ga或其混合物的群组，
以及x为≥0到≤0.5，y为≥0到≤4，z为≥0到≤1以及z1为≥0到≤z。
术语“多相”特别是指和/或包括材料含有形成所述总体成份的至少两种不同结晶学上可分辨的相。这些相可以是不同成分的，但在本发明中这是不需要的。
术语“基本上”特别是指≥95％，优选地≥97％，以及最优选地≥99％的该材料具有期望的成分。
术语“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可控的孔数量或没有任何孔的复合物材料。
术语“多晶材料”从本发明的意义上说特别是指和/或包含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的单晶畴组成，每个畴直径大于0.5μm并可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。
对于本发明内的宽范围的应用，这种材料已经示出具有以下优点至少其一：
-与现有技术的很多“单相”材料相比，该材料的量子效率往往大幅提高，
-该材料通常具有非常良好的转换效率，
-该材料通常具有非常高的热稳定性，特别是光热稳定性。
开始成分中x的增大被认为会增大在烧结之后多相陶瓷中第二相的量，这会增大发光陶瓷的光散射。然而，通过适当地调整额定成分M2-zCezSi5-x-y-(z-z1)Ay+(z-z1)N8-4x-y+z1O4x+y-z1的x值(如上所述)，可以实现表现出由于富氧相的助熔动作的高密度以及高的光学传输的陶瓷。根据优选实施例，x为≥0.0005且≤0.25，优选地≥0.005且≤0.1。
而且认为随着本发明材料中A的含量增加，第二相的含量通常减少，并且材料中O的溶解度增加。对于A包括硼或铝的情形，还经常发现相的颗粒生长(稍后描述)会增加。根据优选实施例，y+(z-z1)为≥0.01且≤0.8，优选地≥0.04且≤0.5。
发明人还发现随着Ba含量的增加，活化剂(Eu和/或Ce)发射经常朝更短波长偏移，而Ca和/或Sr可以导致朝更长波长偏移。优选地，Ba含量(单位是“M”原子数目的％)为≥30％，优选地≥50％。
根据优选实施例，本发明材料包括Eu。如果Eu存在，尤其优选的是其含量(单位是“M”原子数目的％)为≥0.05％且≤5％，优选地≥0.3％且≤2.5％。
然而，如果本发明材料包括Eu和Ce，尤其优选的是Eu和Ce的附加浓度(单位是整个材料的mol％)为≤3％，优选地≤2％。
根据本发明的优选实施例，该多相材料包括成分M2-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1的至少一种相，M、A、z和z1如上文定义且a为从≥0到≤4。
这已被表明对于本发明内的许多应用是有利的。更具体地说，优选地该多相材料包括成分BabMI 2-b-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1的至少一种相，MI选自包括Sr、Ca、Mg、Eu或其混合物的群组，以及A、z和z1如上文定义且a为从≥0到≤4且b为从≥0到≤1。
优选地，材料中M2-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1和/或BabMI 2-b-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1相的体积含量为≥70％，优选地≥80％且最优选地≥90％。
根据本发明的优选实施例，该多相材料包括成分MSi7N10的至少一种相，M如上文定义。
这已表明对于本发明内的许多应用是有利的，特别是由于发现如果该相存在于本发明材料内，则材料的可行性通常大幅简化(easened)(如将在稍后描述)。
优选地MSi7N10相的体积含量为≤15％，优选地≤10％且最优选地≤5％。
根据本发明的优选实施例，该多相材料包括成分M2SiO4的至少一种相，M如上文定义。
这已表明对于本发明内的许多应用是有利的，特别是由于发现如果该相存在于本发明材料内，则材料的可行性通常大幅简化(如将在稍后描述)。
优选地M2SiO4相的体积含量为≤15％，优选地≤10％且最优选地≤5％。
根据本发明的优选实施例，本发明的相的至少之一基本上以颗粒形式存在于多相材料中。
根据本发明的优选实施例，至少一部分颗粒的d50为≥0.5μm到≤4μm。这样一来，对于许多应用，本发明多相陶瓷的照明特征以及稳定性可以改善。
术语“d50”从本发明的意义上为针对平均粒子尺寸的度量，并定义如下：相应样品中粒子(例如颗粒)的数量的50％的尺寸等于或者小于给定的d50值。
根据本发明的附加和/或优选实施例，至少一部分颗粒的d50为≥5μm到≤30μm。这样一来，对于许多应用，本发明多相陶瓷的照明特征以及稳定性可以改善。
注意根据上文，优选的是，颗粒尺寸“相当低”或者“相当高”。因此清楚的是，如果一些颗粒“小”(即具有0.5到4μm的d50)并且一些颗粒“大”(即具有从5到30μm的d50)，则颗粒的混合物也是本发明的优选实施例。
根据本发明的优选实施例，在陶瓷材料用10W/cm2的光功率密度和2.75eV的平均光子能量在260℃暴露10小时之后，陶瓷多相材料的光热稳定性为≥95％到≤100％。
术语“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。术语不受影响特别是表示所发射光的强度保持恒定。
根据本发明的优选实施例，在陶瓷材料用10W/cm2的光功率密度和2.75eV的平均光子能量在260℃暴露10小时之后，陶瓷多相材料的光热稳定性为≥85％到≤97％，优选地≥95％到≤99％。
根据本发明的优选实施例，陶瓷多相材料的热导率为≥0.07Wcm-1K-1到≤0.3W cm-1K-1。
根据本发明一个实施例，陶瓷多相材料示出对于从≥550nm到≤1000nm波长范围内的光在空气中垂直入射时≥10％到≤85％的透明度。
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优选地是在≥20％到≤80％，对于波长范围从≥550nm到≤1000nm的光，更优选地是在≥30％到≤75％以及最优选地是在＞40％到＜70％。
术语“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波长的入射光的≥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(在任意角度)而言，透射穿过该样品。该波长优选地在≥550nm且≤1000nm的范围内。
根据本发明的优选实施例，陶瓷多相材料具有为理论密度的≥95％且≤101％的密度。在此上下文中，多相陶瓷的所有相对密度特别是指一般成分M2-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1和/或BabMI 2-b-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1的优选主要组成部分的理论密度。
根据本发明的优选实施例，陶瓷多相材料具有为理论密度的≥97％且≤100％的密度。
根据本发明所描述的优选实施例，低于100％的密度优选地是通过将陶瓷烧结到其中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，陶瓷基体中总的孔的体积在≥0.2％至≤2％范围内。优选平均孔径在≥400nm至≤1500nm范围内。
本发明还涉及由至少两种前驱体材料制作用于根据本发明的发光器件的陶瓷多相材料的方法，这至少两种前驱体材料包括M2Si5-yAyN8-yOy材料和硅前驱体材料。
术语“硅前驱体材料”特别是指或者包括含有硅酸盐或取代的硅酸盐的材料。特别优选的是硅酸盐和/或氧氮硅酸盐。最优选的是MSi2O2N2和/或M2SiO4。
优选地该方法包括低温挤压步骤，优选地处于＜100℃的温度，最优选地处于环境温度。
令人惊奇地发现，根据本发明的材料可以无高温挤压步骤而被制造。
术语“挤压步骤”特别是指和/或包括含有前驱体材料(如果需要，包含另外的辅助剂或补充材料)的混合物受＞50bar的压力至少＞30分钟。
根据本发明的另一实施例，该方法包括烧结步骤，该烧结步骤优选地在挤压步骤之后进行。
术语“烧结步骤”从本发明的意义上说特别是指在热影响下致密化前驱体粉末而不达到烧结材料的主要组成的液态，这可以与单轴或等静压的应用相结合。
根据本发明的优选实施例，烧结步骤为无压的(pressureless)，优选地在还原或惰性气氛中。
根据本发明的优选实施例，该方法进一步包含，在烧结之前，将陶瓷前驱体材料挤压到为材料主要组成的相应单晶相的其理论密度的≥50％到≤70％，优选地≥55％到≤65％的步骤。在实践中已经示出，这改善了用于如结合本发明所述的大多数陶瓷多相材料的烧结步骤。
根据本发明的优选实施例，制作用于根据本发明的发光器件的陶瓷多相材料的方法包含下述步骤：
(a)混合用于陶瓷多相材料的前驱体材料
(b)可选地煅烧前驱体材料，优选地在≥1300℃到≤1700℃的温度，以除去挥发性材料(诸如在使用碳酸盐情况下的CO2)
(c)可选地研磨和清洗
(d)第一挤压步骤，优选的是使用具有期望形状(例如，杆状或丸状)模具的合适的粉末压实工具的单轴挤压步骤，和/或优选地在≥3000bar到≤5000bar的冷等静压步骤。
(e)烧结步骤，在≥1500℃到≤2200℃在惰性、还原或略微氧化气氛中，压力为≥10-7mbar到≤104mbar。
(f)可选地，在＞1000℃到＜1700℃在惰性气氛中或在含有氢气氛中的后退火步骤。
根据该方法，对于大多数期望的材料成分，该制作方法已经制作出如本发明中使用的最好的陶瓷多相材料。
根据本发明的发光器件以及如使用本方法制作的陶瓷多相材料可以用于各种各样的系统和/或应用中，以下为它们之中的一种或多种：
-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。
前面提到的组成部分、以及所主张保护的部件和在所述实施例中根据本发明使用的组成部分，就它们的尺寸、形状、材料选择和技术概念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、图和各图及实例的以下描述中披露了本发明的目的的其它细节、特征、特性和优势，其中各图及实例以实例性方式示出根据本发明在发光器件中使用的陶瓷多相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示出存在于根据实例I的材料中的三个主相的三个XRD图案，
图3示出根据本发明实例II的材料的XRD图案，
图4示出存在于根据实例II的材料中的三个主相的三个XRD图案，
图5示出与在制作材料之前加入的前驱体材料的量相关的主相相对含量的图示，
图6分别示出实例I和II的材料的两个发射光谱。
具体实施方式
实例I和II
结合实例I和II一起将更好地理解本发明，实例I和II以纯粹说明性方式地为发明陶瓷多相材料的两个实例。
实例I涉及Ba1.454Sr0.536Eu0.01Si4.967N7.868O0.132，其以如下方式制作：
首先制作两种前驱体材料(a)和(b)：
(a)Ba1.5Sr0.49Eu0.01Si5N8粉末的制备
(Ba0.75Sr0.245Eu0.005)2Si5N8粉末根据下述反应来制备
1.5BaH2+0.49SrH2+5SiN4/3+0.005Eu2O3+2/3N2→
Ba1.5Sr0.49Eu0.01Si5N8+0.015H2O+1.975H2
所有前驱体粉末在干燥气氛中通过球磨混合，随后在形成气体气氛中以1450℃煅烧。在煅烧之后，粉末被碾碎并用盐酸清洗和干燥：粉末A
(b)SrSi2O2N2的制备
SrSi2O2N2根据下述反应来制备
SrO+0.5SiO2+3/2SiN4/3→SrSi2O2N2
所有前驱体粉末在干燥气氛中通过球磨混合，随后在氮气气氛中以1300℃煅烧：粉末B
(c)陶瓷处理
95wt％粉末A与5wt％粉末B在干乙醇中通过球磨混合。在添加聚乙烯醇缩丁醛粘结剂并颗粒化之后，混合物通过冷等静压挤压以获得生陶瓷盘。该盘在氮气气氛中以600℃去粘合并以1650℃在氮气气氛下煅烧4-8小时。
结果：具有4.32g/cm3密度(与纯相(Ba0.75Sr0.25)2Si5N8陶瓷的理论密度相比97.3％的相对密度)的致密复合陶瓷。
实例I的材料的XRD图案示于图1中。图2示出三个XRD图案(从上到下)：M2SiO4(正交)，MSi7N10和M2Si5N8(正交)。
从图1和图2的叠加明显看出，根据实例I的材料包括作为主相(＞90％)的正交M2Si5N8相以及作为附加相的正交M2SiO4和MSi7N10。
实例II
实例II涉及Ba1.404Sr0.582Eu0.014Si4.936N7.744O0.256
该材料与实例I的材料类似地制作，只是在步骤a)中制作具有0.7at％Eu掺杂级(相对于M型原子)的粉末，且在步骤c)陶瓷加工中，90wt％粉末A与10wt％粉末B混合。
结果，获得了具有与纯相(Ba0.75Sr0.25)2Si5N8陶瓷的理论密度相比96.7％的相对密度的致密复合陶瓷。
实例I的材料的XRD图案示于图3中。图4示出三个XRD图案(从上到下)：M2SiO4(正交)、MSi7N10和M2Si5N8(正交)。
从图3和图4的叠加明显看出，根据实例I的材料包括作为主相(＞85％)的正交M2Si5N8相以及作为附加相的正交M2SiO4和MSi7N10。
图5示出更广义的图，该图中示出如在本发明的一些实例中所发现的SrSi2O2N2前驱体材料的量和三个相的相对含量之间的关联。总的说来，M2SiO4和MSi7N10的含量随着SrSi2O2N2前驱体材料的增加的添加量而增加，借此当最初混合物中SrSi2O2N2前驱体材料的量超过5wt％时，通常M2SiO4相更突出。
图6示出实例I和II的材料的发射光谱。
为此，实例I和II的陶瓷厚度为200μm的经过抛光样品使用具有450nm发射的发蓝光的LED光源来激发。陶瓷显示出在琥珀色光谱范围内的有效发射。由于较高的Sr和Eu浓度，与实例I相比，实例II(虚线)显示出红移色点。
在上文详述的实施例中的元件和特征的特殊组合仅为实例性的；这些教导与本文中的和以引用方式结合于此的专利/专利申请中的其它教导的互换和替代也被特意地考虑在内。如本领域技术人员将理解的，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实例的方式，而非意图是限制性的。本发明的范围在下述权利要求及其等同物中限定。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的范围。

Claims (10)

1.一种发光器件，包括光源，特别是LED，以及发光材料，该发光材料为基本上具有下述成分的陶瓷多相材料：
M2-zCezSi5-x-y-(z-z1)Ay+(z-z1)N8-4x-y+z1O4x+y-z1
其中M选自包括Sr、Ca、Ba、Mg、Eu或其混合物的群组，
A选自包括Al、B、Ga或其混合物的群组，
以及x为≥0到≤0.5，y为≥0到≤4，z为≥0到≤1以及z1为≥0到≤z。
2.如权利要求1所述的发光器件，其中x为≥0.0005且≤0.25。
3.如权利要求1或2所述的发光器件，其中y+(z-z1)为≥0.05且≤0.8。
4.如权利要求1至3中任意一项所述的发光器件，其中Ba含量(单位是“M”原子数目的％)为≥30％。
5.如权利要求1至4中任意一项所述的发光器件，其中Eu含量(单位是“M”原子数目的％)为≥0.02％且≤5％。
6.如权利要求1至5中任意一项所述的发光器件，其中Eu和Ce加入的浓度(单位是整个材料的mol％)为≤3％，
7.如权利要求1至6中任意一项所述的发光器件，其中该多相材料包括成分M2-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1的至少一种相，M、A、z和z1如上文定义且a为从≥0到≤4。
8.如权利要求1至7中任意一项所述的发光器件，其中该多相材料包括成分MSi7N10和/或M2SiO4的至少一种相。
9.如权利要求1至8中任意一项所述的发光器件，该材料中M2-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1和/或BabMI 2-b-zCezSi5-a-(z-z1)Aa+(z-z1)N8-a+z1Oa-z1相的体积含量为≥70％以及/或者M2Si7N10相和/或M2SiO4相的体积含量为≤15％。
10.包括如权利要求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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