CN103502179A - 陶瓷磁光材料及其选择方法 - Google Patents

陶瓷磁光材料及其选择方法 Download PDF

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CN103502179A
CN103502179A CN201280021224.XA CN201280021224A CN103502179A CN 103502179 A CN103502179 A CN 103502179A CN 201280021224 A CN201280021224 A CN 201280021224A CN 103502179 A CN103502179 A CN 103502179A
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岛田忠克
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Shin Etsu Chemical Co Ltd
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Abstract

本发明涉及一种陶瓷磁光材料，其特征在于，其包含以下述式(1)所示的氧化物为主成分的氧化物陶瓷，且25℃下的所述氧化物陶瓷晶体的晶界的折射率与主相的折射率之差为0.004以下，(TbxRe1-x)2O3(1)(式中，Re表示选自钪、钇、镧、铕、钆、镱、钬、镥中的至少一种元素，0.4≤x≤1.0)。根据本发明，能够可靠提供偏振光状态良好且消光比大的用于光隔离器的法拉第旋光器等的陶瓷磁光材料，能够提供用于加工机械用光纤维激光器的光隔离器的小型化。

Description

陶瓷磁光材料及其选择方法
技术领域
本发明涉及一种用于构成光隔离器等磁光设备(例如法拉第旋光器)的陶瓷磁光材料及其选择方法。
背景技术
近年来，伴随激光加工机械的发展，利用光和磁的相互作用的磁光设备正在受到关注。其中之一为隔离器，该隔离器为抑制如下现象的装置，即若来自激光光源的振荡的光被途中的光学系统反射并返回光源，则会扰乱来自激光光源的振荡的光而形成不稳定的振荡状态的现象。因此，利用该作用，将光隔离器配置在激光光源和光学部件之间进行利用。
光隔离器具有法拉第旋光器、配置在法拉第旋光器的光入射侧的偏光镜、配置在法拉第旋光器的光射出侧的检偏镜这三个部件。光隔离器利用如下的性质，即在与光的前进方向平行地对法拉第旋光器施加磁场的状态下，若光射入法拉第旋光器，则在法拉第旋光器中偏光面发生旋转，也就是所谓的法拉第效应。即，在入射光中，与偏光镜具有相同偏光面的光通过偏光镜，射入法拉第旋光器。该光在法拉第旋光器中相对于光的前进方向旋转正45度而射出。
与之相对，从与入射方向相反的方向射入法拉第旋光器的返回光在最初通过检偏镜时，仅与检偏镜具有相同偏光面的成分的光通过检偏镜，射入法拉第旋光器。接着，在法拉第旋光器中，返回光的偏光面从最初的正45度进一步旋转正45度，因此，形成与偏光镜正90度的直角的偏光面，返回光无法透过偏光镜。
在作为如上所述的光隔离器的法拉第旋光器使用的材料中，需要法拉第效应大且其使用的波长的透射率要高。
另外，若在射出光内产生与入射的光不同的偏光成分，则由于该不同的偏光成分透过偏光镜，因此返回光的阻断变得不充分。
作为该不同的偏光成分的产生状态的评价，向作为法拉第旋光器使用的材料射入0度～90度的偏振光，并使射出光通过偏光镜后射入光接收器，并通过光接收器对光的强度进行测定，由最大值(Imax)和最小值(Imin)，通过下述式计算消光比(S)并进行评价。
S＝-10log(Imin/Imax)［单位dB］
消光比希望较大，但一般情况要求30dB以上。
在特开2010-285299号公报中，作为韦尔代常数较大的原材料，公开了(TbxRe1-x)2O3：0.4≤x≤1.0的氧化物单晶及透明氧化物陶瓷。
透明氧化物陶瓷与氧化物单晶相比，由于将反应温度抑制为较低，能够通过简单的设备进行大量生产，且廉价，因此，有望用于工业中。
例如在特许第4033451号公报中记载了以通式R2O3(R为稀土类元素)表示的稀土类氧化物，其晶体结构为立方晶且无双折射。因此，通过完全去除气孔及杂质的偏析可获得透明性优良的烧结体。
另外，如特开平5-330913号公报中所示出的，为了去除气孔，添加烧结助剂是有效的。而且，如特许第2638669号公报中也公开了如下方法，在热等静压压制成形工序后进行再烧结，去除气孔。
另一方面，若加入烧结助剂长时间进行热处理，则晶界处产生烧结助剂等的偏析，在一些情况下，晶粒的主相的折射率和晶界的折射率产生差别。
这样，在主相和晶界的折射率产生差别的情况下，透过的光的偏光状态发生变化，具体而言，存在消光比变小，使用该材料制造的光隔离器的光分离度恶化的问题。
发明内容
发明所要解决的课题
本发明的目的在于提供一种偏振光状态良好且消光比大的陶瓷磁光材料及其选择方法。
用于解决课题的手段
本发明人为了解决上述课题反复锐意研究的结果发现，在以韦尔代常数较大且为顺磁性元素的铽氧化物和稀土类(钪、钇、镧、铕、钆、镱、钬及镥)氧化物为主成分，向其添加一种或多种烧结助剂进行混合、成形、煅烧后，在真空下进行烧结，进而，在HIP处理后进行退火处理而制造陶瓷时，对各工序的时间、温度、气氛等条件进行各种改变，对获得的陶瓷的颗粒主相和晶界的折射率差与消光比的关系进行调查，其结果，若折射率差比0.004小，则能够获得烧结助剂等向晶界的偏析也较少，非常均匀，且消光比优良的材料，从而完成了本发明。
因此，本发明提供下面所示的陶瓷磁光材料及其选择方法。
〔1〕一种陶瓷磁光材料，其特征在于，其包含以下述式(1)所示的氧化物为主成分的氧化物陶瓷，且25℃下的所述氧化物陶瓷晶体的晶界的折射率与主相的折射率之差为0.004以下，
(TbxRe1-x)2O3    (1)
式中，Re表示选自钪、钇、镧、铕、钆、镱、钬、镥中的至少一种元素，0.4≤x≤1.0。
〔2〕如〔1〕所述的陶瓷磁光材料，其用于光隔离器的法拉第旋光器。
〔3〕一种消光比大的陶瓷磁光材料的选择方法，其特征在于，从以下述式(1)所示的氧化物为主成分的氧化物陶瓷中，选择25℃下的所述氧化物陶瓷晶体的晶界的折射率与主相的折射率之差为0.004以下的氧化物陶瓷，
(TbxRe1-x)2O3    (1)
式中，Re表示选自钪、钇、镧、铕、钆、镱、钬、镥中的至少一种元素，0.4≤x≤1.0。
〔4〕如〔3〕所述的选定方法，陶瓷磁光材料用于光隔离器的法拉第旋光器。
发明效果
根据本发明，能够可靠提供偏振光状态良好且消光比大的用于光隔离器的法拉第旋光器等的陶瓷磁光材料，并可提供用于加工机械用光纤维激光器的光隔离器的小型化。
附图说明
图1是晶界及主相的折射率测定装置的说明图；
图2是表示位置信息与反射光强度的关系的一个例子的说明图；
图3是表示折射率差与消光比的关系的图表。
具体实施方式
本发明涉及的光隔离器的法拉第旋光器用陶瓷磁光元件，其特征在于，包含以下述式(1)
(TbxRe1-x)2O3    (1)
(式中，Re表示选自钪、钇、镧、铕、钆、镱、钬、镥中的至少一种元素，0.4≤x≤1.0)表示的氧化物为主成分，优选波长1.065μm处的韦尔代常数为0.18min/Oe.cm以上的氧化物陶瓷，25℃下的该氧化物陶瓷晶体的晶界的折射率和晶体主相的折射率之差为0.004以下，优选消光比为25dB以上，更优选为30dB以上，特别优选为35dB以上。
在上述式(1)中，x为0.4以上即可，但优选为0.5～0.9，更优选为0.5～0.7。Re为上述元素，但特别优选Y、Gd。
在该情况下，氧化物陶瓷包含钛、锆、铪、钙等的氧化物、氟化物或氮化物等的烧结助剂，或者可根据需要相对于式(1)的氧化物100质量份含有氧化镁、氧化锶、氧化钡等碱土金属氧化物0.0001～0.01质量份。
上述氧化物陶瓷基本上能够采用特开2010-285299号公报中记载的方法进行制造，以以往使用的一般的方法，以韦尔代常数较大且为顺磁性元素的铽氧化物和稀土类(钪、钇、镧、铕、钆、镱、钬及镥)氧化物为主成分，作为烧结助剂，添加一种或多种例如特开平5-330913号公报等中公开的烧结助剂、特别是钛、锆、铪、钙等的氧化物、氟化物或氮化物等烧结助剂进行混合、成形、预烧后，在真空下烧结，再进行HIP处理。
该情况下，在本发明中，在获得的氧化物陶瓷中，选择采用该氧化物陶瓷的晶体晶界的折射率和晶体主相的折射率的差为0.004以下的陶瓷作为均匀性高、消光比大的陶瓷。
主相和晶界的折射率差的测定由于反射光强度根据折射率而发生变化，因此，通过图1所示的如下的方法求得。
对测定的陶瓷(被测定物)1的端面进行镜面抛光，并将其设置在移动的台2上。该移动台2安装在安装于电机3的滚珠丝杆4上，可进行移动。另外，5为基台。
然后，对上述被测定物1从斜上方照射来自光源6的测定光。测定光经扩束器7扩大后，由反射镜8反射，经物镜9照射到被测定物1上，从而可进行微小区域的测定。另外，测定波长越短则能够测定越微小的区域。然后，反射的光通过光接收器(功率计)10接收并检测强度。
若一边移动被测定物，一边通过检测器观察获得的信号，则在晶界的折射率发生变化的情况下，光接收器的信号发生变化。若将被测定物的折射率设为n，则用R＝(n-1)2/(n＋1)2表示在被测定物和空气的界面处的反射率R。
因此，能够从光接收器的信号的变化量求出折射率。
另外，图2表示来自电机的位置信息与来自功率计的反射光强度的关系的一个例子。
通过测定光学系统，折射率的变化量与光接收器的信号的变化量的关系发生变化，因此，通过贴合已知折射率的材料，并与该贴合面垂直地进行镜面抛光，测定该样品，能够校正两者的关系。
另外，通过将被测定物制成薄片进行显微镜观察，即使目测也可定性评价折射率差。
另外，通过目测比较通过上述的反射光测定了折射率差的标准样品和被假设物，能够进行大致评价。
实施例
下面，示出实施例，对本发明具体地进行说明，但本发明并不限定于下述的实施例。
按摩尔比(40～70％：60～30％)的比例使用各种颗粒尺寸的氧化铽粉末和Y2O3或者Gd2O3粉末，向其中以0.5质量％添加ZrO2、HfO2或TiO2作为烧结助剂，进一步添加有效量的作为分散剂及粘合剂的乙基纤维素和聚乙烯醇后，用球磨机将它们混合，从而获得混合物。接着，通过将上述混合物喷雾干燥，获得粒径几十微米的颗粒。使用上述颗粒，进行模具成形作为一次成形之后，进行CIP作为二次成形，获得成形体。将获得的成形体在大气中于400～1000℃下预烧后，在规定的气氛中于1600～1800℃下烧成(正式烧成)。进而，将获得的烧成体进一步进行HIP处理，并根据需要进行退火处理，从而获得15种陶瓷(尺寸：直径φ为6mm、长度10mm)。对获得的陶瓷测定其晶界的折射率与主相的折射率的折射率差及消光比。结果如图所示。
另外，折射率通过如下方式求出，作为折射计使用“椭圆偏振光测定器”，测定25℃下的布鲁斯特角，求出折射率。另外，消光比的评价通过如下方式计算评价，向作为法拉第旋光器使用的材料射入0度～90度的偏振光，使射出光通过偏光镜后射入光接收器，并通过光接收器测定光的强度，由最大值(Imax)和最小值(Imin)，通过下式计算消光比(S)后进行评价。
S＝-10log(Imin/Imax)［单位dB］
结果示于图3。
可确认通过使折射率差为0.004以下，消光比成为30dB以上，折射率差越小，消光比越提高。
符号说明
1 陶瓷(被测定物)
2 移动台
3 电机
4 滚珠丝杆
5 基台
6 光源
7 扩束器
8 反射镜
9 物镜
10 光接收器

Claims (4)

1.一种陶瓷磁光材料，其特征在于，其包含以下述式(1)所示的氧化物为主成分的氧化物陶瓷，且25℃下的所述氧化物陶瓷晶体的晶界的折射率与主相的折射率之差为0.004以下，
(TbxRe1-x)2O3    (1)
式中，Re表示选自钪、钇、镧、铕、钆、镱、钬、镥中的至少一种元素，0.4≤x≤1.0。
2.权利要求1所述的陶瓷磁光材料，其用于光隔离器的法拉第旋光器。
3.一种消光比大的陶瓷磁光材料的选择方法，其特征在于，从包含以下述式(1)所示的氧化物为主成分的氧化物陶瓷，选择25℃下的所述氧化物陶瓷晶体的晶界的折射率与主相的折射率之差为0.004以下的氧化物陶瓷，
(TbxRe1-x)2O3    (1)
式中，Re表示选自钪、钇、镧、铕、钆、镱、钬、镥中的至少一种元素，0.4≤x≤1.0。
4.权利要求3所述的选择方法，其中，陶瓷磁光材料用于光隔离器的法拉第旋光器。
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