CN101278031A - 具有陶瓷SiAlON材料的发光器件 - Google Patents
具有陶瓷SiAlON材料的发光器件 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 72
- 239000000919 ceramic Substances 0.000 title description 5
- 229910003564 SiAlON Inorganic materials 0.000 claims description 52
- 238000005245 sintering Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 241000894007 species Species 0.000 description 3
- 241001025261 Neoraja caerulea Species 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 239000012700 ceramic precursor Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000904 thermoluminescence Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种发光器件，尤其涉及包含SiAlON材料的LED，对于从≥550nm到≤1000nm波长范围的光，所述SiAlON材料具有≥10％到≤85％的透明度。
Description
技术领域
本发明涉及发光器件，尤其涉及LED领域。
背景技术
包含硅酸盐、磷酸盐(例如，磷灰石)和铝酸盐作为基质材料以及包含作为活性材料添加到基质材料中的过渡金属或稀土金属的磷光体(phosphor)是众所周知的。特别是近年来蓝光LED已经实现应用，正积极探求发展采用这种蓝光LED的白光光源。与现有的白光光源相比，作为白光LED，预期具有较低的能耗和较长的使用寿命，现正正朝着它们在液晶面板背光、室内照明器材、汽车面板背光、投影设备光源等等方面的应用发展。
在目前的LED中，由于α-SiAlON优良的材料和热性能，它们越来越广泛地用作发射体材料。然而，到目前为止对于某些应用，发射光谱以及热发光猝灭性能仍有待提高，尤其是将LED用于汽车应用如车的背光时。
发明内容
本发明的目标是提供包含具有改进的性能的SiAlON材料的发光器件。
通过根据本发明权利要求1的发光器件达到此目标。因此，提供一种发光器件，尤其是LED，包含SiAlON材料，该SiAlON材料对于≥550nm到≤1000nm波长范围的光在空气中垂直入射具有≥10％到≤85％的透明度。
采用这种SiAlON材料时，在大多数应用中可以显著提高发光器件的性能(如在后面将要描述的一些应用中那样)。
优选地，对于≥550nm到≤1000nm波长范围的光，在空气中垂直入射的透明度为≥20％到≤80％，对于从≥550nm到≤1000nm波长范围的光，更优选为≥30％到≤75％，且最优选＞40％到＜70％。
优选地，对于≥650nm到≤800nm波长范围的光，在空气中垂直入射的透明度为≥10％到≤85％，更优选≥20％到≤80％，且最优选≥30％到≤75％。
术语“SiAlON材料”尤其包含和/或包括下列材料：
Mx v+Si12-(m+n)Alm+nOnN16-n，
x＝m/v，且M为金属，优选选自Li、Mg、Ca、Y、Sc、Ce、Pr、Nf、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu或它们的混合物，
以及这些材料与添加剂的混合物，所述添加剂可以在陶瓷加工期间添加。这些添加剂可以完全或部分结合到最终材料中，其因此还可以是几种化学上不同的物种的复合材料(composite)(包埋入组成略有不同的玻璃基质中的SiAlON微晶)并尤其包括所属领域中称为熔剂(flux)的物种。适合的熔剂包括碱土金属或碱金属氧化物和氟化物、SiO2等。
在本发明的意义上，术语“透明”尤其是指对于在空气中垂直入射，不能被材料吸收的某一波长的入射光，≥10％，优选≥20％，更优选≥30％，最优选≥40％且≤85％穿过样品(以任意角度)。所述波长优选在≥550nm和≤1000nm范围内。
根据本发明优选的实施方案，所述SiAlON材料在黄色-琥珀色可见光波长范围内具有最大值为≥570nm到≤640nm的发射谱带(emissionband)。这允许构建具有改进的性能的发光器件。优选地，所述SiAlON材料在黄色-琥珀色可见光波长区域内具有最大值为≥580nm到≤620nm，更优选≥590nm到≤610nm的发射谱带。
根据本发明优选的实施方案，所述SiAlON材料在黄色-琥珀色可见光波长区域内具有半宽度(half-width)为≥50nm到≤180nm的发射谱带。这导致允许进一步改进发光器件的尖锐的发射谱带。优选地，所述SiAlON材料在黄色-琥珀色可见光波长区域内具有半宽度为≥60nm到≤130nm的发射谱带。
根据本发明优选的实施方案，所述SiAlON材料具有理论密度的≥95％到≤100％。通过具有这样的密度，与密度较低的材料相比，所述SiAlON材料显示出显著改进的机械和光学性能。优选地，所述SiAlON材料具有理论密度的≥97％到≤100％，更优选≥98％到≤100％。
根据本发明优选的实施方案，所述SiAlON材料是多晶材料。
在本发明的意义上，术语“多晶材料”特别是指这样一种材料，其具有的体积密度大于主要成分的90％，由超过80％的单晶晶畴(singlecrystal domain)组成，每个晶畴直径大于0.5μm且具有不同的结晶取向(crystallographic orientation)。所述单晶晶畴可以通过无定形或玻璃质材料或通过额外的结晶成分连接。
根据本发明优选的实施方案，所述SiAlON材料是陶瓷材料。
在本发明的意义上，术语“陶瓷材料”尤其是指具有数量受控的气孔或无孔的结晶或多晶致密材料或复合材料。
优选地，所述陶瓷材料的厚度D是30μm≤D≤5000μm，优选60μm≤D≤2000μm，最优选80μm≤D≤1000μm。在实践中已表明这是最适合的。
根据本发明优选的实施方案，在从≥50℃到≤150℃的整个温度范围内，所述SiAlON材料在黄色-琥珀色可见光波长区域内的发射谱带中的最大值和/或半宽度的变化是≥0nm到≤20nm。这样，发光器件在工作期间例如当用于汽车时将表现出稳定的性能。
优选地，在从≥0℃到≤200℃，最优选从≥-40℃到≤250℃的整个温度范围内，所述SiAlON材料在黄色-琥珀色可见光波长区域内的发射谱带中的最大值和/或半宽度的变化是≥0nm到≤20nm。
优选地，在从≥50℃到≤150℃，优选从≥0℃到≤200℃，且最优选从≥-40℃到≤250℃的整个温度范围内，所述SiAlON材料在黄色-琥珀色可见光波长区域内的发射谱带中的最大值和/或半宽度的变化是≥2nm到≤18nm。优选地，在从≥50℃到≤150℃，优选从≥0℃到≤200℃，且最优选在≥-40℃到≤250℃的整个温度范围内，所述SiAlON材料在黄色-琥珀色可见光波长区域内的发射谱带中的最大值和/或半宽度的变化是≥4nm到≤15nm。
根据本发明优选的实施方案，所述SiAlON材料包含铕掺杂的Ca-α-SiAlON作为主要成分，铕掺杂的Ca-α-SiAlON通式为(Ca1-x，Eux)m/2Si12-(m+n)Alm+nOnN16-n，2≤m≤4，0.001≤n≤2且0.01≤x≤0.20。更优选的是2.5≤m≤3.5，0.01≤n≤1且0.015≤x≤0.15的组成。最优选的是2.75≤m≤3.25，0.05≤n≤0.5且0.015≤x≤0.1的组成。
已发现，在大部分的应用中低氧含量和掺杂水平会导致材料发光性能提高。
术语“主要成分”特别是指所述SiAlON材料≥95％，优选≥97％且最优选≥99％由这种材料组成。然而，在一些应用中，在总体组成中也可以存在痕量添加剂。这些添加剂特别地包括诸如熔剂的本领域已知的物种。适合的熔剂包括碱土金属或碱金属氧化物和氟化物，SiO2等及它们的混合物。
根据本发明优选的实施方案，所述SiAlON材料的玻璃相比例是≥2％到≤5％，更优选≥3％到≤4％。实践中已经表明，具有这种玻璃相比率的材料显示出改进的性能，这对本发明是有利且理想的。
在本发明的意义上，术语“玻璃相”尤其是指非晶晶界相(non-crystalline grain boundary phase)，其可以通过扫描电子显微镜或透射电子显微镜检测。
根据本发明优选的实施方案，所述SiAlON材料表面的表面粗糙度RMS(表面平面性的破坏；作为最高和最深的表面特征之差的几何平均数测得)是≥0.001μm且≤100μm。根据本发明的实施方案，所述SiAlON材料表面的表面粗糙度是≥0.01μm且≤10μm，根据本发明的实施方案是≥0.1μm且≤5μm，根据本发明的实施方案是≥0.15μm且≤3μm，以及根据本发明的实施方案是≥0.2μm且≤2μm。
根据本发明优选的实施方案，所述SiAlON材料结构的比表面积是≥10-7m2/g且≤1m2/g。
此外，本发明涉及制备用于根据本发明的发光器件的SiAlON材料的方法，包括烧结步骤。
在本发明的意义上，术语“烧结步骤”特别是指在热的影响下，可结合使用单向压力或等静压力(isostatic pressure)，在无需达到被烧结材料的主要成份的液态的情况下，前体粉末的致密化。
根据本发明优选的实施方案，烧结步骤不加压(pressureless)，优选在还原或惰性气氛中进行。
根据本发明优选的实施方案，该方法进一步包括在烧结前将SiAlON前体材料压制至其理论密度的≥50％到≤70％，优选≥55％到≤60％的步骤。在实践中已表明，这会改进本发明所述的大多数SiAlON材料的烧结步骤。
根据本发明优选的实施方案，制备用于本发明的发光器件的SiAlON材料的方法包括下列步骤：
(a)混合用于SiAlON材料的前体材料
(b)任选地，优选在≥1300℃到≤1700℃温度下焙烧所述前体材料以除去挥发性材料(例如CO2，在采用碳酸盐的情况下)
(c)任选地，研磨和洗涤
(d)第一压制步骤，优选的是使用带有希望形状(例如棒状或丸片状)模具的合适的粉末压紧工具在≥10kN下进行的单向压制步骤，和/或优选在≥3000巴到≤3500巴进行的冷等静压步骤。
(e)在≥1500℃到≤2200℃下进行的不加压烧结步骤
(f)热压步骤，优选的是优选在≥100巴到≤2500巴下并且优选在≥1500℃到≤2000℃温度下进行的热等静压步骤，和/或优选在≥100巴到≤2500巴下并且优选在≥1500℃到≤2000℃温度下进行的热单向压制步骤
(g)任选地，在惰性气氛或空气中在＞1000℃到＜1700℃下进行的后退火步骤。
根据此方法，对于大部分希望的材料组成，这种制备方法生产出最好的在本发明中所用的SiAlON材料。
根据本发明的发光器件以及用本发明的方法制备的SiAlON材料可以用于广泛的***和/或应用中，它们之中的一个或更多如下：
-办公室照明***
-家庭应用***
-商店照明***
-家庭照明***
-重点照明***
-局部照明***
-剧场照明***
-纤维光学应用***
-投影***
-自照明显示***
-像素化显示***
-分段显示***
-警告标志***
-医用照明应用***
-指示器标志***，以及
-装饰照明***
-便携式***
-汽车应用
-温室照明***
上述组分以及要求保护的组分和根据本发明将在所述实施方案中采用的组分，关于它们的尺寸、形状、材料选择以及技术概念无任何特殊例外，可以毫无限制地运用相关领域中已知的选择标准。
附图说明
本发明目标的其它细节、特点及优势公开于从属权利要求、附图和以下对各附图的描述以及实施例中，它们以示例方式显示了用于本发明的发光器件中的SiAlON材料的优选实施方案。
图1显示在20℃和100℃环境温度下根据本发明实施例I的SiAlON材料的LED的发射光谱。
图2显示在1500℃下焙烧后陶瓷前体粉末的X-射线衍射图。
图3显示在1700℃下焙烧后陶瓷丸片的X-射线衍射图。
实施例I：
图1到3涉及Ca0,75Si8,625Al3,375O1,375N14,625:Eu0,25(实施例I)，其按如下所述制备：
由0.751g CaCO3(Alfa Aesar，Karlsruhe，Germany)、1.383g AlN(Nanoamor，Los Alamos，NM，USA)、4.234g无定形Si3N4(Alfa Aesar)以及440mg Eu2O3(Alfa Aesar)合成Ca0,75Si8,625Al3,375O1,375N14,625:Eu0,25。在瓷研钵中混合粉末，填充到钼坩埚中并在形成气体气氛(forming gasatmosphere)中于1500℃焙烧4h。清洗粉末以除去杂质。
碾磨获得的粉末，然后压成丸片，在3200巴下冷静压，并在形成气体气氛中于1700℃烧结4小时。获得的丸片展示出闭合性孔隙，随后在2000巴和1750℃热等静压获得＞99％理论密度的致密陶瓷。
图1显示了在20℃和100℃环境温度下本发明实施例I的SiAlON材料的LED的发射光谱。可以清楚地看出在两个光谱中SiAlON材料的发射最大值都在605nm左右，并且此实施例的SiAlON材料半宽度以及发射最大值的变化＜5nm。
图2显示在1500℃下焙烧后陶瓷前体粉末的X-射线衍射图。图3显示在1700℃下焙烧后陶瓷丸片的X-射线衍射图。在图2中，AlN是作为杂质存在，其导致用星号(“*”)标记的几个谱带，而焙烧后的丸片(图3)基本上是纯的。
在上面详细描述的实施方案中，要素及特征的具体组合仅是示例性的；还明确预期了这些教导与本申请中以及作为参考引入的专利/申请中的其它教导的互换和替代。所属领域技术人员将认识到，所属领域普通技术人员能够想到对本文所述内容进行变化、改进和采用其它实施方式而不脱离本发明所要求保护的主旨和范围。因此，上述描述仅是作为例子而不是试图作为限制。在下列权利要求及其等同描述中限定本发明的范围。此外，在说明书和权利要求中所用的参考标记不限制本发明所要求保护的范围。
Claims (10)
1.发光器件，尤其是包含SiAlON材料的LED，其中所述SiAlON材料对于≥550nm到≤1000nm波长范围的光在空气中垂直入射，具有≥10％到≤85％的透明度。
2.权利要求1的发光器件，其中所述SiAlON材料在黄色-琥珀色可见光范围内具有最大波长为≥570nm到≤640nm的发射谱带。
3.权利要求1或2的发光器件，其中所述SiAlON材料在黄色-琥珀色范围内具有半宽度为≥50nm到≤180nm的发射谱带。
4.权利要求1到3任一项的发光器件，其中所述SiAlON材料具有理论密度的≥95％到≤100％。
5.权利要求1到4任一项的发光器件，其中在从≥50℃到≤150℃的整个温度范围内，在所述SiAlON材料的黄色-琥珀色可见光范围内的发射谱带中的最大波长和/或半宽度的变化是≥0nm到≤20nm。
6.权利要求1到5任一项的发光器件，其中所述SiAlON材料包含作为主要成分的铕掺杂的Ca-α-SiAlON，其通式为(Ca1-x，Eux)m/2Si12-(m+n)Alm+nOnN16-n，2≤m≤4，0.001≤n≤2且0.01≤x≤0.20。
7.权利要求1到6任一项的发光器件，其中所述SiAlON材料的玻璃相比例是≥2％到≤5％。
8.一种制备用于权利要求1到7任一项的发光器件的SiAlON材料的方法，包括烧结步骤。
9.根据权利要求8的方法，进一步包括在烧结前将所述SiAlON前体材料压制至其理论密度的≥50％到≤70％的步骤。
10.一种***，包括根据权利要求1到7任一项的发光器件和/或根据权利要求8到9任一项的方法制备的SiAlON材料，该***用于下列一种或更多种应用：
-办公室照明***，
-家庭应用***，
-商店照明***，
-家庭照明***，
-重点照明***，
-局部照明***，
-剧场照明***，
-纤维光学应用***，
-投影***，
-自照明显示***，
-像素化显示***，
-分段显示***，
-警告标志***，
-医用照明应用***，
-指示器标志***，以及
-装饰照明***，
-便携式***，
-汽车应用，
-温室照明***。
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| CN101663371B (zh) * | 2007-04-20 | 2013-02-06 | 皇家飞利浦电子股份有限公司 | 具有改进的颜色稳定性的白色发光光源和发光材料 |
| ATE510901T1 (de) * | 2007-12-03 | 2011-06-15 | Koninkl Philips Electronics Nv | Lichtemittierende vorrichtung mit einem grünes licht emittierenden material auf sialonbasis |
| EP2231816B9 (en) * | 2007-12-03 | 2012-03-14 | Philips Intellectual Property & Standards GmbH | Ceramic material for leds with reduced scattering and method of making the same |
| TW201000603A (en) * | 2008-02-12 | 2010-01-01 | Koninkl Philips Electronics Nv | Light emitting device comprising a ceramic material with line emitter activators and an interference filter |
| JP2013258037A (ja) * | 2012-06-12 | 2013-12-26 | Panasonic Corp | 照明装置 |
| US10283681B2 (en) * | 2013-09-12 | 2019-05-07 | Cree, Inc. | Phosphor-converted light emitting device |
| JP6222612B2 (ja) * | 2014-03-06 | 2017-11-01 | 地方独立行政法人神奈川県立産業技術総合研究所 | 透明蛍光サイアロンセラミックスおよびその製造方法 |
| US11486550B2 (en) * | 2019-05-22 | 2022-11-01 | Nichia Corporation | Method for producing wavelength conversion sintered body |
| JP7448806B2 (ja) | 2019-05-22 | 2024-03-13 | 日亜化学工業株式会社 | 波長変換焼結体の製造方法 |
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| JP3837551B2 (ja) * | 2003-06-20 | 2006-10-25 | 独立行政法人物質・材料研究機構 | 酸窒化物蛍光体 |
| JP3914987B2 (ja) * | 2003-06-20 | 2007-05-16 | 独立行政法人物質・材料研究機構 | サイアロン蛍光体とその製造方法 |
| KR101102304B1 (ko) * | 2003-08-22 | 2012-01-03 | 도쿠리츠교세이호징 붓시쯔 자이료 겐큐키코 | 산질화물 형광체 및 발광기구 |
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| CN104736664B (zh) * | 2012-10-17 | 2016-09-14 | 宇部兴产株式会社 | 波长转换部件及使用其的发光装置 |
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| US20080220260A1 (en) | 2008-09-11 |
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