CN102344284B - 波长转换元件,发光装置,及制造波长转换元件的方法 - Google Patents

波长转换元件,发光装置,及制造波长转换元件的方法 Download PDF

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CN102344284B
CN102344284B CN201110164946.8A CN201110164946A CN102344284B CN 102344284 B CN102344284 B CN 102344284B CN 201110164946 A CN201110164946 A CN 201110164946A CN 102344284 B CN102344284 B CN 102344284B
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phase
wavelength changing
changing element
light
rare earth
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CN102344284A (zh
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绵谷和浩
塚谷敏彦
高井康
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Shin Etsu Chemical Co Ltd
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Abstract

本发明涉及波长转换元件，发光装置，及制造波长转换元件的方法，特别涉及一种包含(A)石榴石相和(B)钙钛矿、单斜或硅酸盐相的多晶烧结陶瓷，其中相(B)的细晶粒包含并分散在相(A)中，该多晶烧结陶瓷用作波长转换元件。由于透过波长转换元件的光在石榴石相和钙钛矿、单斜或硅酸盐相之间的界面处散射，所以包含该波长转换元件的发光装置产生颜色更为均匀且损失最小的光。

Description

波长转换元件,发光装置,及制造波长转换元件的方法
技术领域
本发明涉及一种与光源共同使用的波长转换元件，该元件可使该光源的一部分光的波长发生转换，同时允许另一部分的光通过，一种利用该元件的发光装置，以及制造该元件的方法。
背景技术
发光二极管是目前可用的最有效的光源之一。进行了有效的努力来通过结合蓝光LED和荧光体开发白光发射装置。例如：JP-A2007-150331公开了一种包括石榴石等的波长转换元件，特别是可透光的、均一波长转换元件，该元件可使发光器件所发光的波长发生转换，以及包括该波长转换元件的发光装置。期望该波长转换元件比现有技术的包括荧光体和在其中分散荧光体的树脂的波长转换层具有更高的耐热性能及更高的机械强度，而且期望该波长转换元件在面对随着发光器件输出功率增大而释放更多的热量时，具有更高的耐久性。
在采用石榴石波长转换元件(其是可透光且均一的)的情况下，由波长转换元件透射的光源的一部分光直接传输通过该波长转换元件，然而被该波长转换元件吸收并转换波长的另一部分光在所有方向上均匀传输。因此透射光和波长转换光有不同的光分布图案。结果，来自于包含这种波长转换元件的发光装置的光输出，缺乏颜色均匀性，并且从该发光装置中只能获得具有变化颜色的照射表面。作为该问题的对策，可将不透明或者半透明的光扩散元件置于发光装置的外部，以减轻照射表面中的可见颜色变化。因为光在穿过扩散元件时产生部分损失，所以采用光扩散元件导致光利用率降低。
引用文件
专利文献1：JP-A2007-150331(US7514721，EP1958269)
发明概述
本发明的目的是提供一种与光源共同使用的波长转换元件，用于使来自该光源的一部分光的波长发生转换，同时允许另一部分光透过，该元件减轻了由透射光和波长转换光之间不同的发光分布导致的可见颜色变化，并能提供具有均匀颜色的照射表面，采用该元件的发光装置，以及制造该元件的方法。
在采用波长转换元件的发光装置中，用于减轻由透射光和波长转换光之间不同的发光分布导致的可见颜色变化的有效方式是，使透射光在波长转换元件内散射，同时最小化透射光的损失。
例如，为了使光线在透过烧结体形式的波长转换元件时散射，可以设想的是有意地降低烧结密度以结合孔或气泡用于减少由发光装置发出光的可见颜色变化。在此尝试中，由于波长转换元件和气泡之间巨大的折射率差异，在元件和气泡之间的界面处发生光的反射和散射。不希望地，发光装置的发光效率降低。
发明人发现在采用包含(A)石榴石相和(B)钙钛矿、单斜或硅酸盐相(其中细晶粒相(B)包含并分散在相(A)中)多晶烧结陶瓷作为构造发光装置的波长转换元件时，穿过波长转换元件传输的光在石榴石相和钙钛矿相、单斜相或硅酸盐相之间的界面处被充分散射，从而减少发光装置所发射光的可见颜色变化，同时使发光装置的发光效率的降低最小化。
一方面，本发明提供了包含多晶烧结陶瓷的波长转换元件，该多晶烧结陶瓷包含(A)石榴石相和(B)至少一种选自钙钛矿、单斜或硅酸盐相中的相，其中相(B)的细晶粒包含并分散在相(A)中。作为相(A)的石榴石相有如下组成式(1)：
(A1-xBx)3C5O12(1)
其中，A是至少一种选自Y、Gd和Lu的稀土元素，B是至少一种选自Ce、Nd和Tb的稀土元素，C是至少一种选自Al和Ga的元素，x是从0.002至0.2的数值。
在优选实施方案中，钙钛矿相包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，及氧；单斜相包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，及氧。硅酸盐相包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，硅和氧。优选地，相(B)的细晶粒具有的平均晶粒尺寸为至少0.1μm。同样优选地，烧结陶瓷具有的孔隙率为至多0.1体积％。
另一方面，本发明提供了包含光源和如上所定义的波长转换元件的发光装置，其中来自光源的一部分光穿过波长转换元件，而来自光源的另一部分光被波长转换元件转换波长，并且这些部分合并以产生光输出。
又一方面，本发明提供了如上所定义的波长转换元件的制造方法，其包括以下步骤：混合第一源粉末和第二源粉末，所述第一源粉末以形成相(A)的组成包含相(A)中所含的元素；所述第二源粉末以形成相(B)的组成包含相(B)中所含的元素；将粉末混合物成型为成形体，并加热该成形体用以烧结。
发明有益效果
由于传输穿过波长转换元件的光在石榴石相和钙钛矿相、单斜相或硅酸盐相之间的界面处散射，因此包含该波长转换元件的发光装置产生颜色更均匀且损失最小化的光输出。由于相对于现有技术，透射光和波长转换光之间的分布均匀性得到改善，因此包含该波长转换元件的发光装置提供了具有最小化的可见颜色变化的照射表面。
附图简要说明
图1示意地示出了波长转换元件，其中相(B)包含并分散在相(A)中。
图2示出了实施例1中得到的波长转换元件的电子显微图和EPMA图像。
图3示出了实施例2中得到的波长转换元件的电子显微图和EPMA图像。
图4示出了实施例3中得到的波长转换元件的电子显微图和EPMA图像。
图5示出了比较例1中得到的波长转换元件的电子显微图和EPMA图像。
具体实施方式
本发明中的波长转换元件包含多晶烧结陶瓷，该多晶烧结陶瓷包含(A)石榴石相和(B)至少一种选自钙钛矿相、单斜相和硅酸盐相中的相。在波长转换元件中，相(B)形成的细晶粒或晶体包含并分散在作为主相的相(A)形成的晶体中。
从图1中的波长转换元件的横截面示意图中可以看出，这些相的状态以相(B)至少一种选自钙钛矿相、单斜相和硅酸盐相的相的细晶粒2分散和分布在相(A)即石榴石相的晶体(基体)1中的结构存在。两种不同的相形成所谓的海中岛(island-in-sea)的结构。
波长转换元件中包含这种相结构的多晶烧结陶瓷。当在发光装置中采用波长转换元件来适合产生光输出，使得来自该光源的一部分光穿过波长转换元件，而另一部分被波长转换元件转换波长的光，透过波长转换元件的光和被波长转换元件所转换的光都在石榴石相和钙钛矿相、单斜相或硅酸盐相之间的界面处充分散射。这减少了来自发光装置光输出的可见颜色变化，同时使发光装置发射效率的降低最小化。
相(B)与相(A)的比例即B/A优选从0.001至0.2，更优选从0.001至0.1。如果比例B/A超过该范围，发射效率可能降低。如果比例B/A低于该范围，则用于改善可见颜色变化的散射效果可能降低。通过在制备烧结体的过程中，控制对应于各自相的源粉末的比例，可以将比例B/A设置在该范围之内。
相(B)的细晶粒或晶体具有的平均晶粒尺寸优选为至少0.1μm，同时优选至高1mm。当晶粒尺寸小于0.1μm，透射光的散射效果可能会减弱。超过1mm的晶粒尺寸具有如此大的晶粒尺寸引起透射光的损失的可能性。
同样优选地，烧结陶瓷具有的孔隙率为至多0.5体积％，更优选至多0.1体积％。超出这个范围的孔隙率具有这种可能：透过波长转换元件的光和由波长转换元件的吸收和转换波长的光被散射进波长转换元件的孔内并由此损失，导致发光放率的降低。
在本发明的波长转换元件中，作为相(A)的石榴石相优选为具有如下组成式(1)的石榴石相：
(A1-xBx)3C5O12(1)
其中，A是至少一种选自Y、Gd和Lu的稀土元素，B是至少一种选自Ce、Nd和Tb的稀土元素，C是至少一种选自Al和Ga的元素，x是从0.002至0.2的数值。
另一方面，作为相(B)钙钛矿相优选为氧化物钙钛矿相，其包含至少一种选自Ce、Nd和Tb的稀土元素，更优选为一种钙钛矿相，其包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，及氧。具体地，钙钛矿相具有如下组成式(2)：
(A1-yBy)CO3(2)
其中A、B和C如上所定义，y是从0.002至0.98的数值。
同样作为相(B)的单斜相优选为氧化物单斜相，其包含至少一种选自Ce、Nd和Tb的稀土元素，更优选为这样的单斜相，其包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，及氧。具体地，单斜相具有如下组成式(3)：
(A1-zBz)4C2O9(3)
其中A、B和C如上所定义，z是从0.002至0.98的数值。
同样作为相(B)的硅酸盐相优选为这样的硅酸盐相，其包含至少一种选自Ce、Nd和Tb的稀土元素，更优选为这样的硅酸盐相，其包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，硅和氧。
优选采用烧结技术制备多晶陶瓷的波长转换元件，这是因为具有相(B)可以均匀分散在相(A)中的优势，尽管它可采用其他任何技术制备。
在通过烧结技术的制备中，具有含量比或组成对应于或接近于石榴石相的陶瓷粉末，是以包含足够形成相(A)组成的相(A)元素的源粉末形式制备的。其通过以下步骤制备：混合氧化物、氢氧化物和其它形式的包含于石榴石相中的元素的粉末以获得需要的含量比，并且在环境气氛或真空中，于900至1,500℃温度下烧制混合物10分钟至8小时。由此得到形成石榴石相的单一相组分的源粉末。
包含足够形成相(B)的组分的相(B)元素的源粉末以如下方式制备。当相(B)是钙钛矿或单斜相，如同石榴石相的情况一样，具有的含量比或组分对应于或接近于钙钛矿相的陶瓷粉末，或具有比或组分对应于或接近于单斜相的陶瓷粉末，是通过以下步骤制备的：混合的包含在相关相中的元素的氧化物和其它形式粉末，以获得需要的含量比，并且在环境气氛或真空中，于900至1500℃温度下烧制混合物10分钟至8小时。由此得到形成相关相的单一相组分的源粉末。
当相(B)是硅酸盐相时，可将含硅化合物，例如氧化硅或有机硅树脂的粉末用作相(B)的源粉末。据认为，当具有组成式(1)的石榴石相应用为相(A)时，在烧结过程中，所添加的部分或者全部硅化合物形成了由元素A、B和C(以式(1))和硅和氧构成的硅酸盐相。
然后，将用于形成相(A)的源粉末和用于形成相(B)的源粉末混合，以便提供如上所述的比例B/A。将得到的粉末混合物通过压制，粉浆浇铸或片材化技术成型。将获得产物加热并在环境气氛、还原气氛或真空中烧制至致密的陶瓷烧结体，以作为波长转换元件。尤其是，为了最小化波长转换元件中的气泡，真空烧结是优选的。
为了增大波长转换元件的密度，烧结温度优选是至少1,700℃，更优选是至少1,750℃。烧结温度优选高于2,000℃。超过以上范围的烧结温度是经济上有缺点的。烧结时间通常为约4至约24小时。在烧结步骤中，不仅形成作为主相的相(A)，而且形成相(B)，且相(B)分散于相(A)中。
实施例
通过说明而非限制的方式给出了本发明中的实施例。
实施例1
在混合器中，将平均颗粒尺寸为1.0μm的99.9％纯度的氧化钇Y2O3粉末，平均颗粒尺寸为0.5μm的99.0％纯度的氧化铝Al2O3粉末，和平均颗粒尺寸为0.2μm的99.9％纯度的氧化铈CeO2粉末，以摩尔比Y∶Al∶Ce＝2.98∶5∶0.02进行组合并混合30分钟，得到500g粉末混合物。将粉末混合物在1,400℃的环境气氛中烧制4h，得到形成石榴石相的单一相组分的源粉末(1-1)500g。
分别地，将平均颗粒尺寸为1.0μm的99.9％纯度的氧化钇Y2O3粉末，平均颗粒尺寸为0.5μm的99.0％纯度的氧化铝Al2O3粉末，和平均颗粒尺寸为0.2μm的99.9％纯度的氧化铈CeO2粉末，以摩尔比Y∶Al∶Ce＝2.98∶3.00∶0.02混合，获得1g粉末混合物。粉末混合物在1400℃的环境气氛中烧制4h，得到形成钙钛矿相单一相组分的1g源粉末(1-2)。
将源粉末(1-1)和(1-2)在混合器中混合1h，得到用于烧结的源粉末(1)。将源粉末(1)经过单轴模压机模压，并在1750℃下真空烧结，得到致密烧结体。从烧结体切出1.5mm长、2.0mm宽、200μm厚的条带，准备将其用作波长转换元件。
该波长转换元件经过测量具有的烧结密度为4.55g/cm3，孔隙率为0.1vol％。在波长转换元件的横截面中的观测表明该致密烧结体中几乎没有气泡。用XRD定性分析了波长转换元件，确认主相由YAG相(石榴石相)和存在的YAP相(钙钛矿相)组成。波长转换元件的电子显微观察和电子探针显微分析(EPMA)证实结构为，平均晶粒尺寸为约3μm的YAP相晶粒，以YAP相晶粒被包含且分散在YAG相中的状态存在于YAG相中。图2显示了电子显微图和EMPA图像。
当波长转换元件被470nm的光激发时，显示内部量子效率为0.90。同样，当波长转换元件中的一个表面被470nm的点光源照射时，在照射表面的相对表面上，它产生没有可见颜色变化的发光。
实施例2
通过如同实施例1的步骤获得源粉末(1-1)，500g。分别地，将平均颗粒尺寸为1.0μm的99.9％纯度的氧化钇Y2O3粉末，平均颗粒尺寸为0.5μm的99.0％纯度的氧化铝Al2O3粉末，和平均颗粒尺寸为0.2μm的99.9％纯度的氧化铈CeO2粉末，以摩尔比Y∶Al∶Ce＝3.98∶2.00∶0.02混合，获得1g粉末混合物。将粉末混合物在1,400℃的环境气氛中烧制4h，得到形成单斜相单一相组分的1g源粉末(2-2)。
将源粉末(1-1)和(2-2)在混合器中混合1h，得到用于烧结的源粉末(2)。源粉末(2)经过单轴压制机模压，1,750℃下真空烧结，得到致密烧结体。从烧结体切出1.5mm长、2.0mm宽、200μm厚的条带，将其准备用作波长转换元件。
该波长转换元件经过测量具有的烧结密度为4.55g/cm3，孔隙率为0.1vol％。在波长转换元件的横截面中的观测表明该致密烧结体中几乎没有气泡。用XRD定性分析了波长转换元件，确认主相由YAG相(石榴石相)和存在的YAM相(单斜相)组成。波长转换元件的电子显微观察和EPMA证实结构为，具有平均晶粒尺寸为约5μm的YAM相晶粒，以YAM相晶粒被包含且分散在YAG相中的状态存在于YAG相中。图3显示了电子显微图和EPMA图像。
当波长转换元件被470nm的光激发时，显示内部量子效率为0.92。同样，当波长转换元件中的一个表面被470nm的点光源照射时，在光照表面的相对表面上，它产生没有可见颜色变化的发光。
实施例3
在混合器中，将平均颗粒尺寸为1.0μm的99.9％纯度的氧化钇Y2O3粉末，平均颗粒尺寸为0.5μm的99.0％纯度的氧化铝Al2O3粉末，和平均颗粒尺寸为0.2μm的99.9％纯度的氧化铈CeO2粉末，以摩尔比Y∶Al∶Ce＝2.99∶5∶0.01进行组合并混合30分钟，得到粉末混合物。将粉末混合物在1,400℃下环境气氛中烧制4h，得到形成石榴石相单一相组分的源粉末(1-1)。
将一定数量氧化硅粉末添加到源粉末(1-1)中，以便提供2000ppm的含量，并且在混合器中混合一小时，得到100g用于烧结的源粉末(3)。源粉末(3)经过单轴压制机模压，1,780℃下真空烧结，产生致密烧结体。从烧结体切出1.5mm长、2.0mm宽、200μm厚的条带，将其准备用于制备波长转换元件。
该波长转换元件经过测量具有的烧结密度为4.54g/cm3，孔隙率为0.2vol％。在波长转换元件的横截面中的观测表明该致密烧结体中几乎没有气泡。用XRD定性分析了波长转换元件，确认主相由YAG相(石榴石相)和存在的硅酸盐相组成。波长转换元件的电子显微观察和EPMA证实结构为，平均晶粒尺寸为约5μm的硅酸盐相晶粒，以硅酸盐相晶粒被包含且分散在YAG相中的状态存在于YAG相中。图4显示了电子显微图和EPMA图像。
当波长转换元件被470nm的光激发时，显示内部量子效率为0.92。同样，当波长转换元件中的一个表面被470nm的点光源照射时，在被照射面的相对表面上，它产生没有可见颜色变化的发光。
比较例1
通过如同实施例1的步骤源粉末(1-1)，500g。然后，将所得源粉末(2)经过单轴压制机模压，1,750℃下真空烧结，产生致密烧结体。从烧结体切出1.5mm长、2.0mm宽、200μm厚的条带，将其准备用作波长转换元件。
该波长元件经过测量具有的烧结密度为4.55g/cm3，孔隙率为0.1vol％。用XRD定性分析了波长转换元件，它是由石榴石相组成。电子显微观察和EPMA显示波长转换元件的结构为除了石榴石相不可观察到其它相。图5显示了电子显微照片和EPMA图像。
当波长转换元件被470nm的光激发时，显示内部量子效率为0.90。同样，当波长转换元件中的一个表面被470nm的点光源照射时，在照射表面的相对表面上，它产生可见颜色变化的发光。

Claims (7)

1.包含多晶烧结陶瓷的波长转换元件，该多晶烧结陶瓷包含：
(A)具有组成式(1)的石榴石相：
(A1-xBx)3C5O12(1)
其中，A是至少一种选自Y、Gd和Lu的稀土元素，B是至少一种选自Ce、Nd和Tb的稀土元素，C是至少一种选自Al和Ga的元素，x是从0.002至0.2的数值，和
(B)选自单斜相和硅酸盐相的至少一种相，其中
相(B)的每一细晶粒包含在相(A)的晶体基体中并分散在相(A)的晶体基体中。
2.权利要求1中的波长转换元件，其中单斜相包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，及氧。
3.权利要求1中的波长转换元件，其中硅酸盐相包含至少一种选自Y、Gd和Lu的稀土元素，至少一种选自Ce、Nd和Tb的稀土元素，至少一种选自Al和Ga的元素，硅和氧。
4.权利要求1中的波长转换元件，其中相(B)的细晶粒具有至少0.1μm的平均晶粒尺寸。
5.权利要求1中的波长转换元件，其中烧结陶瓷具有至多0.1％体积的孔隙率。
6.发光装置，包含光源和权利要求1中的波长转换元件，其中来自光源的一部分光穿过波长转换元件，而来自光源的另一部分光被波长转换元件转换波长，并且这些部分合并以产生光输出。
7.一种用于制备权利要求1中的波长转换元件的方法，该方法包括以下步骤：
混合第一源粉末和第二源粉末，所述第一源粉末以形成相(A)的组成包含相(A)中所含的元素，所述第二源粉末以形成相(B)的组成包含相(B)中所含的元素；
将粉末混合物成型为成形体，并
加热该成形体以烧结。
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