CN110832054A - 发光陶瓷和波长转换装置 - Google Patents

发光陶瓷和波长转换装置 Download PDF

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CN110832054A
CN110832054A CN201880041950.5A CN201880041950A CN110832054A CN 110832054 A CN110832054 A CN 110832054A CN 201880041950 A CN201880041950 A CN 201880041950A CN 110832054 A CN110832054 A CN 110832054A
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luminescent ceramic
light
sample
wavelength conversion
ceramic
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CN110832054B (zh
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吴竹悟志
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Murata Manufacturing Co Ltd
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Abstract

本发明提供一种不易产生光劣化的发光陶瓷。所述发光陶瓷是由烧绿石型化合物构成的，相对于通式M1XM2YM3ZOW100摩尔％含有0.01摩尔％以上的Bi，通式中，M1为选自La、Y、Gd、Yb和Lu中的至少1种的元素，M2为选自Zr、Sn和Hf中的至少1种的元素，M3为选自Ta、Nb和Sb中的至少1种的元素，X、Y、Z和W为保持电中性的正数，其中，在X+Y+Z＝2.0的情况下，0.005≤Z≤0.2，3X+4Y+5Z为7.02以下。

Description

发光陶瓷和波长转换装置
技术领域
本发明涉及发光陶瓷和使用了该发光陶瓷的波长转换装置。
背景技术
以往，已知有一旦被光照射则射出波长与所照射的光不同的光的发光陶瓷。下述的专利文献1中记载的发光陶瓷通过在还原气氛中对以ABOW(其中，A含有选自La、Y、Gd、Yb和Lu中的至少一种，B含有选自Zr、Sn和Hf中的至少一种和Bi，W为用于保持电中性的正数)所示的烧绿石型化合物为主成分的陶瓷进行热处理而得到。
另外，下述的专利文献2中记载了如果荧光体长时间暴露于能量密度高的光中，则发光量逐渐降低。
现有技术文献
专利文献
专利文献1：WO2014/119416 A1
专利文献2：日本特开2012-62394号公报。
发明内容
如专利文献2中的记载，如果荧光体长时间暴露于能量密度高的光中，发光量逐渐降低。该现象被称为光劣化或光退色。照明用途等中，在长时间内始终要求一定的发光量、发光颜色。因此，要求不能产生这样的光劣化。
对于专利文献1中记载的发光陶瓷ABOW，长期间使用时也产生光劣化。特别是如果暴露于波长短且能量密度高的光中，则存在发光量逐渐降低的问题。
本发明的目的在于提供一种不易产生光劣化的发光陶瓷和波长转换装置。
本发明的发光陶瓷是由烧绿石型化合物构成的，相对于通式M1xM2YM3ZOW100摩尔％含有0.01摩尔％以上的Bi，通式中，M1为选自La、Y、Gd、Yb和Lu中的至少1种的元素，M2为选自Zr、Sn和Hf中的至少1种的元素，M3为选自Ta、Nb和Sb中的至少1种的元素，X、Y、Z和W为保持电中性的正数，其中，在X+Y+Z＝2.0的情况下，0.005≤Z≤0.2，3X+4Y+5Z为7.02以下。
本发明的发光陶瓷的3X+4Y+5Z优选为6.92以上。此时，不仅不易产生光劣化，还不具有潮解性。
本发明的发光陶瓷的Z优选为0.02以上，更优选为0.05以上。此时，进一步不易产生光劣化。
本发明的发光陶瓷优选相对于上述通式M1xM2YM3ZOW100摩尔％，以5摩尔％以下的比例含有上述Bi。
应予说明，在本说明书中，只要没有特别说明，元素的含量摩尔％为相对于M1xM2YM3ZOW100摩尔％的比例。
本发明的波长转换装置具备由本发明构成的发光陶瓷和对上述发光陶瓷照射紫外线的光源。
应予说明，本申请的“发光陶瓷”是指在照射紫外线等光时，吸收所照射的光的能量的至少一部分，并以与所照射的光的波长不同的波长的光的形式放射所吸收的能量的陶瓷。
根据本发明，能够提供一种即使暴露于激发光的光中，也不易产生光劣化的发光陶瓷和具有该发光陶瓷的波长转换装置。
附图说明
图1是表示实验例中准备的No.1和No.4的发光陶瓷的XRD衍射图谱的图。
图2是表示使用了No.1和No.5的发光陶瓷的情况下的发光强度的经时变化的图。
图3是表示No.17和No.18的发光陶瓷的XRD衍射图谱的图。
图4是表示作为本发明的一实施方式的波长转换装置的示意结构图。
具体实施方式
以下，参照附图对本发明的详细内容和本发明的具体实施方式进行说明。
应予指出，本说明书中记载的各实施方式是例示性的，在不同的实施方式之间，可以进行构成的部分置换或组合。
本发明的发光陶瓷是相对于通式M1xM2YM3ZOW100摩尔％含有0.01摩尔％以上的Bi的由烧绿石型化合物构成的发光陶瓷，通式中，M1为选自La、Y、Gd、Yb和Lu中的至少1种的元素，M2为选自Zr、Sn和Hf中的至少1种的元素，M3为选自Ta、Nb和Sb中的至少1种的元素，X、Y、Z和W为保持电中性的正数，在X+Y+Z＝2.0的情况下，0.005≤Z≤0.2，3X+4Y+5Z为7.02以下。
本发明的发光陶瓷是通过对具有上述组成比的陶瓷材料进行煅烧，在此之后在还原气氛中进行热处理而得到的。
本发明的发光陶瓷为陶瓷，因此与单晶的发光材料相比容易制造。在上述煅烧中，上述陶瓷材料可以直接以粉末状进行煅烧，也可以暂时成型为规定形状后进行煅烧。不论是哪种情况均是通过在还原气氛中进行热处理而得到发光陶瓷。发光陶瓷可以是粉末状，也可以分散于树脂、玻璃等。粉末状、分散于树脂或玻璃的状态均能够作为用于制成具有波长转换功能的元件的材料而使用。
本发明的发光陶瓷M1xM2YM3ZOW为烧绿石型化合物。本发明中，只要可以看到X射线衍射中的超晶格峰即(311)或(331)的峰，即为烧绿石型化合物。
本发明的发光陶瓷中，3X+4Y+5Z优选为6.92以上。在该情况下，由于发光陶瓷不具有潮解性，因此可以提供一种适合于波长转换装置等的发光陶瓷。
另外，上述通式的Z优选为0.02以上，更优选为0.05以上，在该情况下，进一步不易产生光劣化。
本发明中，相对于上述通式M1xM2YM3ZOW所示的化合物100摩尔％，含有0.01摩尔％以上的Bi。Bi优选含有0.05摩尔％以上。由此，能够进一步提高发光的量子产率。优选为以5摩尔％以下的比例含有Bi。由此，能够进一步提高发光的量子产率。更优选为以3摩尔％以下含有Bi，进一步优选为以1摩尔％以下的范围含有。
应予说明，为了得到本发明的发光陶瓷，优选使用Bi2O3作为Bi源。
另外，在本发明的发光陶瓷中，优选厚度为1mm时的波长450nm～800nm的透光率为50％。更优选为60％以上，进一步优选为70％以上。由此，能够提供一种透光性进一步提高的进一步适合于波长转换装置、照明等的发光陶瓷。
另外，在本发明的发光陶瓷中，优选照射激发光时得到的发光量子产率为40％以上，更优选为50％以上，进一步优选为60％以上。
(发光陶瓷的制造方法)
对本发明的发光陶瓷的制造方法进行说明。
首先，将陶瓷原料粉末成型为规定的形状，得到作为陶瓷材料的未煅烧的陶瓷成型体。接下来，在含有氧的气氛中对未煅烧的陶瓷成型体进行煅烧。由此，得到陶瓷M1xM2YM3ZOW。
用于得到陶瓷M1xM2YM3ZOW的煅烧气氛优选氧浓度为98体积％以上。煅烧温度(最高温度)例如可以为1500℃～1800℃左右。煅烧工序的煅烧温度(最高温度)保持时间例如可以为5小时～100小时左右。
接下来，在还原气氛中对得到的陶瓷M1xM2YM3ZOW进行热处理。由此，得到上述发光陶瓷。上述还原气氛没有特别限定，例如，可以使用H2/H2O气氛。热处理时的温度(最高温度)例如优选为800℃～1200℃，更优选为900℃～1100℃。另外，热处理温度(最高温度)的保持时间例如可以为1小时～100小时左右。
发光陶瓷的波长400nm～600nm的透光率通过上述热处理而提高。煅烧时产生的空穴成为色心，吸收波长400nm～600nm的波长的光。与此相对，利用上述还原气氛中的热处理，使成为色心的空穴，因还原前的从氧侧提供的电子中和，由此提高了透光率。
本发明的发光陶瓷由M1xM2YM3ZOW表示，但可以包含M1、M2、M3和O以外的不可避免地混入的杂质即不可避免的杂质。作为不可避免的杂质的例子，可举出SiO2、B2O3、Al2O3等。
(波长转换装置的实施方式)
图4是表示作为本发明的一实施方式的波长转换装置的示意结构图。
波长转换装置6用于照明等，包括波长转换部1和光源2。波长转换部1由本发明的发光陶瓷构成。光源2产生紫外线。在基板4上设置有光源2。以包围光源2的周围、并且包围从光源2射出的紫外线的光轴的方式，在基板4上配置反光板3。波长转换部1固定于反光板3的光射出侧端部，在与光源2间隔的位置与光源2对置。作为光源2，例如可以使用LED等。
驱动时，从光源2朝向波长转换部1照射激发光。激发光的一部分被反光板3反射而到达波长转换部1。波长转换部1被激发光激发而发光。
应予说明，对波长转换装置6进行说明，但本发明的波长转换装置并不限于图4所示的波长转换装置6，也可以是具有由本发明的发光陶瓷构成的波长转换部和使该发光陶瓷射出光的光源的各种形态的波长转换装置。
(实验例)
接着，通过描述本发明的发光陶瓷的实验例，对本发明进一步进行详细说明。应予说明，本发明并不限于以下的实验例。
以下，通过举出本发明的具体实验例，对本发明更具体地进行说明。
(实验例1)
作为原料，准备La(OH)3、Gd2O3、Y2O3、Yb2O3、Lu2O3、ZrO2、HfO2、SnO2、Nb2O5、Ta2O5、Sb2O3和Bi2O3。称量这些原料，以得到下述的表1的摩尔比所示的组成，利用球磨机进行20小时湿式混合。使得到的混合物干燥后，在1300℃下焙烧3小时，得到焙烧物。将得到的焙烧物与水和有机分散剂一起置入球磨机，进行12小时湿式粉碎。使用得到的粉碎物，利用湿式成型法，成型为直径30mm和厚度5mm的圆盘状的形状。将得到的成型物埋入由与该成型物相同的组成构成的粉体中，在氧气氛下(约98体积％氧浓度)，利用1700℃的温度煅烧20小时。由此得到烧结体。
将得到的烧结体利用晶体切割器切割成5mm见方×厚度1.2mm的矩形板状的形状。对利用切割得到的矩形板状的烧结体在N2/H2/H2O混合气体气氛(氧分压：1.7×10-13MPa)中进行热处理。热处理时的温度、即最高温度为1000℃，1000℃下的保持时间为3小时。对上述热处理的矩形板状的烧结体的两面以厚度成为0.5mm的基板的方式进行镜面研磨，制成评价用的样品。
如上所述，得到下述的表1所示的No.1～No.14的样品。应予说明，表1的加料组成比为摩尔比。另外，使该摩尔比标准化以使X+Y+Z＝2.0。
另外，M1为3价离子，M2为4价离子，M3为5价离子，由此以使这些阳离子的总电荷不与烧绿石型化合物的通式A2B2O7矛盾的方式设定X、Y和Z各值。实验例1中，以满足3X+4Y+5Z＝7.0或其附近的方式，设定X、Y、Z各值。
另外，为了得到上述评价用的样品，基于中途得到的焙烧物的组成，来分析所使用的XRF组成。其结果得到作为目标的组成的烧结体，确认了在组成中成分没有显著挥发。
另外，对于得到的评价用样品，进行XRD分析。图1示出样品No.1和样品No.4的XRD衍射图谱。由图1可知，样品No.1和样品No.4均大致为烧绿石结构单相。图1中，代表性地示出了样品No.1和样品No.4的结果，但确认了其它样品也大致为烧绿石结构单相。
另外，对于得到的各样品，使用绝对PL量子产率测定装置(Hamamatsu Photonics株式会社制，产品编号：C9920-02)，测定激发波长365nm下的发光量子产率。将结果示于下述的表1。
另外，各样品具有透明性。使用紫外可视分光光度计(株式会社岛津制作所社制，产品编号：UV-2500PC)对各样品的直线透过率测定700nm下的直线透过率。下述的表1中一并示出直线透过率。
(光劣化的评价)
对于得到的评价用的样品，使用光致发光测定装置(西进商事株式会社制)，对样品表面照射120分钟波长325nm和输出10mW的He-Cd激光。测定由此时的样品得到的发光强度的经时变化。发光强度的检测波长为580nm。图2中作为测定结果的例子示出了样品No.1和样品No.5的发光强度的经时变化。由图2明确可知，发光强度的降低在光照射开始后数分钟内特别显著，之后降低量随时间变小，显示饱和的趋势。本实验例中，利用相对发光强度评价各样品的光劣化。这里，相对发光强度是指照射120分钟后的发光强度与照射之后的发光强度的比例。将这样测定的相对发光强度一并示于下述的表1。
由表1可知，对于Z＝0的样品No.1，量子产率为80％以上，并且直线透过率为70％以上。即，样品No.1是透明度高、透光率优异的发光陶瓷。然而，相对发光强度小于0.7，样品No.1中，显著产生光劣化。
另一方面，对于含有Ta作为5价离子的Z＝0.005～0.200的样品No.3～样品No.7，相对发光强度均为0.75以上。即可知能够抑制光劣化。另外，将样品No.3～样品No.7的组成与样品No.1的组成进行比较时，除了Ta的有无之外，样品No.3～样品No.7的La多，Zr少。
但是，根据样品No.9和样品No.10的结果可知，若仅是组成中的La、Zr的构成比率发生变化，则对光劣化的特性没有影响。因此，根据上述结果可知，使用5价离子Ta对光劣化的抑制有效。
另外，根据样品No.2的结果可知，如果Z为0.002以下，则光劣化的抑制效果变小，不优选。另外，根据样品No.8的结果可知，若Z为0.400以上，则量子产率、透光率降低，因而不优选。因此，优选地，Z多于0.002，优选为小于0.400的范围，进一步优选为0.005～0.200。在该情况下，量子产率和透光率良好，并且能够有效抑制光劣化。
另外，根据样品No.11和样品No.12的结果可知，通过使用5价离子的Ta带来的光劣化抑制的程度，即使在Bi的加料量增减的情况下也不受影响。
根据样品No.13和样品No.14的结果可知，在相对于M1XM2YM3ZOW100摩尔％Bi含有比例为0.0300摩尔％的样品No.13、Bi含有比例为0.0500摩尔％的样品No.14中，虽然与上述的样品No.4、11和12相比量子产率略降低，但相对发光强度显示足够的值。
(实验例2)
与实验例1同样地，得到下述的表2、表3和表4所示的样品No.15～样品No.42的评价用样品。
对于得到的各评价用样品，与实验例1同样地求出量子产率、直线透过率和相对发光强度。将结果示于下述的表2、表3和表4。应予说明，表2、表3和表4的加料组成比为摩尔比，是以成为X+Y+Z＝2.0的方式标准化的值。另外，与实验例1同样以满足3X+4Y+5Z＝7.0或其附近的方式设定X、Y和Z各值。在下述的表2、表3和表4中也一并示出X、Y和Z的值。
Figure BDA0002330984430000091
对于表2的样品No.15～样品No.18，示出了Ta作为5价离子Z＝0.050时的阳离子的总电荷即3X+4Y+5Z偏离7.000时的结果。根据样品No.15的结果可知，如果总电荷成为7.040以上，则量子产率、直线透过率降低，因此不优选。根据样品No.18的结果可知，若总电荷为6.900，则量子产率和直线透过率高，光劣化少。但如样品No.17和样品No.18的图3所示的XRD衍射图谱中示出的那样，如果总电荷为6.900以下，则在样品中残存未反应的La。因此，样品显示潮解性，因此不优选。因此，阳离子的总电荷的3X+4Y+5Z优选为6.92以上。
另外，上述总电荷优选为7.02以下。
Figure BDA0002330984430000111
对于表3所示的样品No.19～样品No.22，示出5价离子使用Nb、Sb、或Ta、Nb和Sb的组合的情况下的结果。由表3可知，在使用Nb、Sb的情况下，或者使用这些5价离子元素的组合的情况下，能够有效抑制光劣化。
对于表4的样品No.23～样品No.42，示出作为M1、M2和M3的元素而使用各种元素的情况或者组合这些元素使用的情况的结果。由表4可知，即使M1为La以外时，M2为Zr以外时，M3为Ta以外时，如果Z为0.005～0.200，则进一步能够有效地抑制光劣化。另外，总电荷即3X+4Y+5Z优选为6.92以上，由此能够进一步有效地抑制光劣化。另外，如果3X+4Y+5Z为7.02以下，则能够有效抑制光劣化。
附图标记的说明
1…波长转换部
2…光源
3…反光板
4…基板
6…波长转换装置

Claims (6)

1.一种发光陶瓷，由烧绿石型化合物构成，相对于通式M1xM2YM3ZOW100摩尔％含有0.01摩尔％以上的Bi，通式中，M1为选自La、Y、Gd、Yb和Lu中的至少1种的元素，M2为选自Zr、Sn和Hf中的至少1种的元素，M3为选自Ta、Nb和Sb中的至少1种的元素，X、Y、Z和W为保持电中性的正数，
其中，在X+Y+Z＝2.0的情况下，0.005≤Z≤0.2，3X+4Y+5Z为7.02以下。
2.根据权利要求1所述的发光陶瓷，其中，3X+4Y+5Z为6.92以上。
3.根据权利要求1或2所述的发光陶瓷，其中，Z为0.02以上。
4.根据权利要求3所述的发光陶瓷，其中，Z为0.05以上。
5.根据权利要求1～4中任一项所述的发光陶瓷，其中，相对于所述通式M1xM2YM3ZOW100摩尔％，以5摩尔％以下的比例含有所述Bi。
6.一种波长转换装置，具备：
权利要求1～5中任一项所述的发光陶瓷；和
对所述发光陶瓷照射紫外线的光源。
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