CN104822638A - 透光性铋取代稀土类铁石榴石型烧成体以及磁性光学装置 - Google Patents

透光性铋取代稀土类铁石榴石型烧成体以及磁性光学装置 Download PDF

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CN104822638A
CN104822638A CN201380062945.XA CN201380062945A CN104822638A CN 104822638 A CN104822638 A CN 104822638A CN 201380062945 A CN201380062945 A CN 201380062945A CN 104822638 A CN104822638 A CN 104822638A
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bismuth
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CN104822638B (zh
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渡边聪明
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Abstract

一种透光性铋取代稀土类铁石榴石型烧成体、及使用该烧成体的磁性光学装置，所述透光性铋取代稀土类铁石榴石型烧成体为可用R3-xBixFe5O12表示的烧成体且其特徵在于：平均结晶粒径为0.3μm～10μm，其中R为选自由Y及镧系元素组成的组中的至少1种元素；X为0.5以上且2.5以下的数。

Description

透光性铋取代稀土类铁石榴石型烧成体以及磁性光学装置
技术领域
本发明涉及透光性铋取代稀土类铁石榴石型烧成体，尤其涉及其平均结晶粒径为0.3μm～10μm的透光性铋取代稀土类铁石榴石型烧成体，及使用该烧成体作为磁性光学元件的磁性光学装置。
背景技术
在进行光通信或光测量时，从半导体激光器射出的光在传输路经的途中所设置的部件表面反射，如果该反射光返回到半导体激光器，则激光振荡会变得不稳定。因此，为了遮断这种反射回光，一直以来使用利用使偏光面进行非相反旋转的法拉第转子的光隔离器。另外，同样地，使用利用法拉第转子并按通信路经分别对光的行进方向进行控制的光循环器。
作为上述法拉第转子，以往，一直使用通过液相磊晶法(LPE法)在石榴石基板上生长的铋取代稀土类铁石榴石膜。上述石榴石基板是指Gd3Ga5O12或将其中部分元素取代后的基板，NOG(信越化学公司制)及SGGG(圣戈班公司制)市面上有售。
然而，上述制造方法中存在以下问题：由于所能得的培养膜的组成受基板的晶格常数的制约，(1)在以基于Bi的取代量为首的材料组成的研究中没有自由度；(2)根据基板形状，培养膜的形状受到限制；(3)需要在膜的培养中所使用的昂贵的白金坩埚，及用于将基板保持于液相中的白金支架。
因此，也有研究提出通过固相反应法培养膜(专利文献1及2)，不过，在此种情况下，虽然就法拉第旋转系数而言能够得到所期望的特性，但由于插入损耗及消光性能不能满足要求，至今仍未达到实用水平。
现有技术文献
专利文献
专利文献1日本专利特开平8-91998
专利文献2日本专利特开昭63-35490
发明内容
为了利用固相反应法获得插入损耗和消光性能充分的法拉第转子，本发明人进行了深入的研究，结果发现，固相反应中的反应时间与构成膜材料的平均粒径、以及在光通信和光测量等中所利用的波长范围中的消光性能和插入损耗有关，同时还发现，通过控制固相反应中的反应时间，能够使消光性能(35dB以上)和插入损耗(1.0dB以下)达到使用范围的数值，从而促成了本发明。
即，本发明涉及透光性铋取代稀土类铁石榴石型烧成体及以使用该烧成体作为磁性光学元件为特征的磁性光学装置，所述透光性铋取代稀土类铁石榴石型烧成体的特征在于，其为可用R3-xBixFe5O12表示的烧成体，并且其平均结晶粒径为0.3μm～10μm(其中，R为选自由Y及镧系元素组成的组中的至少1种元素；X为0.5以上且2.5以下的数。)
发明的效果
本发明的透光性铋取代稀土类铁石榴石型烧成体通过固相反应得到，不需要在膜的培养中所使用的昂贵的白金坩埚及用于将基板保持在液相中的白金支架，因此廉价，同时由于无需为了膜的生长使用特殊基板，所以还具有制造适性优良的特别效果。
附图说明
图1是示出本发明的法拉第转子的结构例的图。
图2是示出本发明的光隔离器的结构例的图。
图3是示出本发明的铋取代稀土类铁石榴石型烧成体中的铋取代量和晶格常数之间的关系的图。
具体实施方式
以下，基于实施例对本发明进行详细说明。不过，本发明不受这些实施例所限定，应理解为：本技术领域的技术人员根据这些记载所能进行的单纯的设计变更也包含于本发明之中。
实施例1
将下表1中所示的铋取代稀土类铁石榴石成分进行混合，冷均压(coldisostatic pressing，CIP)成型之后，用真空加热炉进行预烧成。接着，在1150℃～1460℃下施以热均压(hot isostatic pressing，HIP)，得到直径10mm×厚度(t)2mm的黑色烧成体。
表1
试验组成
对两表面进行研磨加工，使用X射线绕射仪确认到，工件具有以R3-xBixFe5O12表示的石榴石构造(参照表2、表3及图3)。其中，R为选自由Y及镧系元素组成的组中的至少1种元素；X为0.5以上且2.5以下的数。
表2
石榴石构造的确认(●石榴石构造，×混有其他构造物)
表3
石榴石基板晶格常数
(LPE法中通常采用的石榴石基板及其晶格常数)
从表2及图3可以清楚地确认，即便是在采用石榴石基板的现有的LPE法中由于基板的晶格常数的限制而无法培养厚膜的X＝1.5和2.0、2.5的组成范围，在本发明的铋取代稀土类铁石榴石烧结体中也能得到厚度为2mm的石榴石构造。
实施例2
对于在实施例1中得到的10mm×(t)1.2mm的烧成体Gd1.5Bi1.5Fe5O12，在1200℃～1350℃下进行追加热烧成，对两面进行研磨之后施以蚀刻并确认了粒径。接着，对工件进一步进行研磨加工，调整其厚度以使法拉第旋转角度为45deg。对该工件的两表面实施对波长1310nm光的对空气无反射涂层(通称：AR涂层)(参照图1)，并测定工件的法拉第旋转角度(作为每单位长度的旋转角度的法拉第旋转系数)、消光性能以及插入损耗。
需要说明的是，平均粒径(以后，称为粒径)是以将如下作业重复三次而得到的数据为基础求出的。即，对工件的表面实施蚀刻处理，观察SEM像并确认在任意直线上的粒子数。结果如表4所示。
表4
Gd1.5Bi1.5Fe5O12组成下的特性
※约45deg
实施例3
除了取代在实施例1中得到的10×mm(t)2mm的烧成体Gd1.5Bi1.5Fe5O12而使用在实施例1中得到的10mm×(t)2mm的烧成体Tb1.5Bi1.5Fe5O12以外，使其他条件与实施例2完全相同，得到了表5所示的结果。
表5
Tb1.5Bi1.5Fe5O12组成下的特性
※约45deg
实施例4
为了确认烧成时间对粒径及性能的影响，将实施例3中实施的1200℃的追加热烧成时间延长5小时、10小时及15小时，其结果如表6所示。
表6
Tb1.5Bi1.5Fe5O12组成下的特性
※约45deg
实施例5
除了取代在实施例4中使用的烧成体Tb1.5Bi1.5Fe5O12而使用烧成体Gd1.5Bi1.5Fe5O12以外，使其他条件与实施例4完全相同，得到了表7所示的结果。
表7
Gd1.5Bi1.5Fe5O12组成下的特性
※约45deg
从表5及表6的结果可以确认，即便温度相同，如果烧成时间不同则粒径也不同。另外，比较表4和表6及表5和表7可知，粒径与插入损耗及消光比之间存在相关关系，为了得到插入损耗1.0dB以下、消光比35dB以上的结果，粒径必须为0.3μm～10μm。
实施例6
除了将AR涂层改为对780nm光的对空气对应的无反射涂层以外，使其他条件与实施例5相同并进行5小时追加热烧成，得到了如表8所示的结果。
表8
Gd1.5Bi1.5Fe5O12组成下的特性
＝>780nm下，45deg，1.5dB/43dB
(-12000deg/cm)
实施例7
使用所得到的工件中的插入损耗小的工件(表7中以1220℃追加烧成5小时的制品)，将工件的厚度研磨成168μm，以使对1310nm光的法拉第旋转角度为45度，并在两表面实施AR涂层后切割成1mm的方块，插入固定在SmCo制的磁铁中。准备2个在金属支架中结合固定了偏振光玻璃的工件，以偏振光玻璃的透过偏振光方向的相对角度成为45度的方式，将所述工件安装固定于上述磁铁的两端，由此制作了光隔离器。如此得到正方向插入损耗为0.25dB，反方向插入损耗与39dB的良好结果(参照图1及图2)。需要说明的是，上述相对角度45度，是指从隔离器的入射侧向出射侧观察时，入射侧的偏振光玻璃的透过偏振光方向与出射侧偏振光玻璃的透过偏振光方向的角度在逆时针方向上相差45度的配置。
同样，将工件的厚度研磨成250μm，以使对1550nm光的法拉第旋转角度为45度，并在两表面实施AR涂层后切割成1mm的方块插入固定在SmCo制的磁铁中，以相对角度为45度的方式将偏振光玻璃固定于两端，从而制作了光隔离器。结果得到了正方向插入损耗为0.20dB，反方向插入损耗为38dB的良好结果。
实施例8
使用所得到的工件中的法拉第旋转系数高的工件(在表7中在1220℃下追加烧成5小时的制品)，将工件的厚度研磨成38μm，以使在780nm的波长范围法拉第旋转角度为45度，并在两表面实施了AR涂层。然后，切割成1mm的方块，以与实施例3同样的方法，制作了波长780nm用的光隔离器。得到了正方向的插入损耗为1.8dB，反方向的插入损耗为42dB的良好结果。
需要说明的是，本发明的法拉第转子与采用以往的LPE法制作的工件相比，插入损耗略高。可以认为这是由于石榴石组成中的一部分Fe离子从Fe3+变为了Fe4+、Fe2+等所引起的。因此，可以推断，通过在气体环境中对制作材料进行退火处理来修正Fe离子的价数，或预先于原料组成中投入能降低Fe离子的价数变动的元素，能够减少插入损耗。另外，还可以认为，通过用Al或Ga等取代Fe这种通常在LPE法中采用的方法能够对在制作组成下的饱和磁场强度进行调整。如本实施例所示，粒径能够通过改变烧成温度和烧成时间来控制，不过也可以通过于原料组成中混入微量的Si或Ge、Al、Zr等影响透明陶瓷制作时的粒径的元素来控制。
由于本发明的透光性铋取代稀土类铁石榴石型烧成体的材料组成无需考虑基板的晶格常数、大小等的影响，因此使大型板状(譬如100×200mm等)的成型加工变成容易，并且，能够高效率地工业性提供在光通信和光测量中所采用的使偏波面进行非相反旋转的材料，即法拉第转子、光隔离器、光循环器等的磁性光学装置，所以本发明在工业上极为有用。
符号说明
1：铋取代稀土类铁石榴石型烧成体
2：反射防止膜(AR涂层)
3：SUS环
4：偏振光玻璃支架
5：偏振光玻璃
6：磁铁
10：法拉第转子
20：光隔离器

Claims (6)

1.一种透光性铋取代稀土类铁石榴石型烧成体，其为可用R3-xBixFe5O12表示的烧成体，且其特征在于：平均结晶粒径为0.3μm～10μm，其中R为选自由Y及镧系元素组成的组中的至少1种元素；X为0.5以上且2.5以下的数。
2.如权利要求1所述的透光性铋取代稀土类铁石榴石型烧成体，其中粒径为0.3μm～10μm。
3.一种磁性光学装置，其特征在于：使用如权利要求1所述的透光性铋取代稀土类铁石榴石型烧成体作为磁性光学元件。
4.如权利要求3所述的磁性光学装置，其中所述透光性铋取代稀土类铁石榴石型烧成体的对1310nm的光的正方向的插入损耗为1.0dB以下，消光比为35dB以上。
5.如权利要求3所述的磁性光学装置，其中所述透光性铋取代稀土类铁石榴石型烧成体的对1550nm的光的正方向的插入损耗为1.0dB以下，消光比为35dB以上。
6.一种透光性铋取代稀土类铁石榴石型烧成体的制造方法，所述透光性铋取代稀土类铁石榴石型烧成体的插入损耗小，且为可用R3-xBixFe5O12表示的烧成体，所述透光性铋取代稀土类铁石榴石型烧成体的制造方法的特征在于包括：通过在气体环境中对所制作的烧成体进行退火处理来修正Fe离子的价数的步骤；和/或预先于所述烧成体的原料组成中添加降低Fe离子的价数变动的元素的步骤。
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