CN111868007A - Cr：YAG烧结体 - Google Patents

Cr：YAG烧结体 Download PDF

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CN111868007A
CN111868007A CN201980018765.9A CN201980018765A CN111868007A CN 111868007 A CN111868007 A CN 111868007A CN 201980018765 A CN201980018765 A CN 201980018765A CN 111868007 A CN111868007 A CN 111868007A
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sintered body
yag
light
yag sintered
atomic ppm
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CN111868007B (zh
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三上充
山崎芳树
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Jks Metal Co ltd
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Abstract

一种Cr：YAG烧结体，其特征在于，所述Cr：YAG烧结体含有Al、Y、Cr、Ca、Mg、Si和O，并且该烧结体中的成分含量满足下述1)～3)的条件式。其中，在条件式中，各元素符号表示成分含量(原子ppm)。1)|(Y+Ca)/(Al+Cr+Si+Mg)‑0.6|＜0.001；2)0原子ppm≤(Ca+Mg)‑(Cr+Si)≤50原子ppm；3)50原子ppm≤Si≤500原子ppm。本发明的实施方式的课题在于提供一种透光性优异并且Cr4+转化率高的Cr：YAG烧结体及其制造方法。

Description

Cr：YAG烧结体
技术领域
本发明涉及Cr：YAG(钇铝石榴石)烧结体及其制造方法。
背景技术
YAG(钇铝石榴石)为包含钇和铝的复合氧化物(Y3AlsO12)的石榴石结构的晶体。以往已知：1)通过在YAG中添加稀土元素中的从原子序数57的Ce至原子序数70的Yb的元素而使构成YAG的“Y元素”进行置换固溶；或者2)通过在YAG中添加过渡金属中的从原子序数22的Ti至原子序数28的Ni的元素而使构成YAG的“Al元素”进行置换固溶，由此置换后的元素成为发光中心并且具有强荧光，并且使用其制作了荧光体、激光介质等。
作为经常使用的材料，有添加了Nd(钕)的Nd：YAG，其是以1064nm的波长发生激光振荡的材料。另外，有将Nd：YAG和添加了四价Cr原子(以下记载为Cr4+)的YAG组合而成的材料，虽然其吸收波长1064nm的光，但是通过调节浓度以使得以一定程度的光量吸收达到饱和(可饱和吸收体)，最初，Cr4+：YAG吸收光，抑制Nd：YAG的激光振荡并蓄积激发量，在此期间，当Cr4+：YAG吸收达到饱和时，一下子产生从在Nd：YAG中所蓄积的激发状态的激光振荡，从而产生强脉冲激光，然后Cr4+：YAG中的吸收状态缓和并返回初始状态，通过反复进行这样的过程，能够形成周期性地产生强脉冲光的、被称为被动调Q振荡的状态。
像这样基于Nd：YAG与Cr：YAG的组合的激光器自动地产生强脉冲光，因此被用于各种用途(例如专利文献1)中。另外，近年来，使用与制作以往的陶瓷时同样的成型、烧结的方法来制作尽可能抑制了存在于晶界处的孔隙(空隙)的多晶YAG，已知该多晶YAG显示出略差于单晶但优异的透射特性。在此，作为涉及多晶YAG烧结体的发明，例如可以列举专利文献2、3。
现有技术文献
专利文献
专利文献1：日本特开2017-201662号公报
专利文献2：日本专利第4237707号
专利文献3：日本专利第5019380号
发明内容
发明所要解决的问题
本发明的实施方式的课题在于提供一种透光性优异并且Cr4+转化率高的Cr：YAG烧结体及其制造方法。
用于解决问题的手段
本发明的实施方式的Cr：YAG烧结体的主旨在于，所述Cr：YAG烧结体含有Al、Y、Cr、Ca、Mg、Si和O，并且该烧结体中的成分含量满足下述1)～3)的条件式。其中，在条件式中，各元素符号表示成分含量(原子ppm)。
1)|(Y+Ca)/(Al+Cr+Si+Mg)-0.6|＜0.001
2)0原子ppm≤(Ca+Mg)-(Cr+Si)≤50原子ppm
3)50原子ppm≤Si≤500原子ppm
发明效果
根据本发明的实施方式，能够制造透光性优异并且Cr4+转化率高的Cr：YAG烧结体。
附图说明
图1为表示对于实施例1和Cr3+：YAG的K吸收边的XANES测定结果的图。
图2为表示将图1中的5990eV附近进一步放大后的图。
图3为用于确认被动调Q功能的激光装置的结构图。
图4为表示实施例1的被动调Q功能的确认结果的图。
具体实施方式
在Cr：YAG中，Cr原子进入YAG中置换了Al原子的位点，但由于Al为三价，因此容易形成同样三价的Cr原子(以下记载为Cr3+)。Cr4+的浓度不足时，难以发生被动调Q，因此期望提高Cr4+的比率。为了使Cr3+成为Cr4+，可以考虑添加二价的原子并利用该二价的原子置换三价的Y原子和三价的Al原子，从而进行价数补偿。但是，并非只要是二价的元素就全都能够实现该价数补偿，目前已知的仅为Ca和Mg。
但是，仅通过将Ca、Mg添加到YAG烧结体中无法得到足够的烧结性，增加添加量时，反而存在烧结性变差、无法得到透光性的问题。本发明人对能够显著提高烧结性的各种添加元素中的Si进行了研究，结果得到了如下发现：由于Si为四价，因此添加Si时，朝阻碍转化为Cr4+的方向起作用，但是通过适当调节Si的量，能够在不阻碍转化为Cr4+的情况下显著地提高烧结性。
鉴于上述发现，本发明的实施方式的Cr：YAG烧结体的特征在于，所述Cr：YAG烧结体含有Al、Y、Cr、Ca、Mg、Si和O，并且该烧结体中的成分含量满足下述1)～3)的条件式。其中，式中，各元素符号表示成分含量(原子ppm)。
1)|(Y+Ca)/(Al+Cr+Si+Mg)-0.6|＜0.001
2)0原子ppm≤(Ca+Mg)-(Cr+Si)≤50原子ppm
3)50原子ppm≤Si≤500原子ppm
关于条件式1)，YAG(组成式：Y3Al5O12)偏离Y：Al＝3∶5的组成比时，有时Al2O3、YAlO3等其它结构的组织析出从而使透光性降低，在这样的情况下，在被动调Q中有时激光振荡停止。因此，要求包含与“Y原子”置换的Ca、与“Al原子”置换的Cr、Mg、Si在内的烧结体的组成比为(Y+Ca)：(Al+Cr+Mg+Si)＝3∶5，即使产生组成偏差，只要在|(Y+Ca)/(Al+Cr+Si+Mg)-0.6|＜0.001的范围内，就能够得到足够的透光性。
本发明的实施方式的Cr：YAG烧结体基本上为四价的Cr置换YAG，并且为了Cr的价数补偿而包含二价的Ca和Mg，为了提高烧结性而还包含Si。Ca具有促进Cr4+转化的作用，但是有时使烧结性变差。另外，Mg也能够微弱地促进Cr4+转化，但是无法充分提高烧结性。此外，对于Si而言，通过添加Si能够提高烧结性，但是由于价数为四价，因此会阻碍Cr4+转化。
在考虑到上述各添加元素的作用和效果时，通过满足上述2)的条件式，能够在利用Ca和Mg促进Cr4+转化的同时，利用Si抑制由Ca引起的烧结性的降低，另外，能够在利用Si提高烧结性的同时，利用Ca、Mg抑制由Si引起的Cr4+转化的阻碍。另一方面，通过添加50原子ppm以上的Si，能够得到提高烧结性的效果，但是Si含量大于500原子ppm时，烧结性变差，因此Si含量如上述3)的条件式所示。
在本发明的实施方式中，Cr：YAG烧结体的波长1300nm的光的透射率优选为80％以上。透光性差时，有时激光被遮蔽从而激光振荡停止。烧结性与透光性存在相关性，在充分进行了烧结的情况下，残留在内部且使光散射的气孔(孔)变少，能够得到透射性优异的烧结体。需要说明的是，在透射率的测定中，透射率根据厚度而变化，因此将烧结体的厚度设定为1cm。
另外，在本发明的实施方式中，转化率Cr4+/(Cr3++Cr4+)优选为0.25以上。这是因为，Cr4+的浓度低时，不发生被动调Q，虽然发生激光振荡，但是不发生脉冲振荡。需要说明的是，如后述所详细说明的，从Cr3+到Cr4+的价数转变的评价可以使用X射线近边吸收光谱(XANES)通过与作为参考试样的Cr3+：YAG烧结体的比较来进行。
接着，对本发明的实施方式的多晶YAG烧结体的制造方法的一例进行说明。
(关于原料粉末)
准备Y2O3粉末、Al2O3粉末、Cr2O3粉末、MgO粉末和CaCO3粉末作为原料，以达到规定的摩尔比的方式进行称量。这些原料粉末优选使用平均粒径为0.3μm～10μm的原料粉末，另外，对于Y2O3粉末、Al2O3粉末而言，优选使用纯度4N以上的原料粉末，对于Cr2O3粉末、MgO粉末、CaCO3粉末而言，优选使用纯度2N以上的原料粉末。
(关于混合)
将上述Y2O3粉末、Al2O3粉末、Cr2O3粉末、MgO粉末和CaCO3粉末投入混合粉碎机中，利用以水为溶剂、以氧化铝为介质的球磨机进行4小时～6小时的湿式混合。此时，为了抑制由原料粉末的聚集而导致的混合不均，优选添加适量的分散剂。在混合后，向从混合粉碎机中取出的浆料中添加Si(OC2H5)4和乳酸铝并进行搅拌。通过该Si(OC2H5)4的添加量能够调节最终的YAG烧结体中的Si含量。
(关于造粒、成型)
接着，将搅拌后的浆料干燥，然后利用筛强制过筛，或者进行喷雾干燥而制作造粒粉，将其放入模具(例如，φ150mm×40mm)中，进行冷压，然后在150MPa～200MPa下进行CIP成型。
(关于预加热)
接着，在大气炉中，为了除去水分而将该成型体在100℃～300℃下加热4小时～6小时，然后为了除去有机成分等而将该成型体在800℃～1000℃下加热1小时～3小时。
(关于烧结、HIP)
接着，将该成型体在1700℃～1900℃下烧结10小时～20小时。此时，在含有氮气的气氛中进行烧结时，由于氮气残留在烧结体中而导致密度降低，因此优选在真空、还原性气氛或者不含有氮气的氧气气氛中进行烧结。然后，在Ar等惰性气氛下、在1600℃～1800℃、100MPa～200MPa下进行HIP(热等静压)1小时～4小时。
(关于退火)
然后，在大气炉中将上述得到的烧结体在1300℃～1500℃下加热5小时～15小时。通过以上操作，能够得到所期望的Cr：YAG烧结体。
包含实施例、比较例在内的本发明的实施方式的Cr：YAG烧结体的评价方法等可以如下所述进行。
(关于成分组成)
关于烧结体中所含的成分组成，通过利用ICP(电感耦合等离子体)发射光谱分析法等进行研究来进行分析。
(关于透光性)
关于透光性，研究没有由Cr产生的吸收的波长1300nm的光的透射率。如果在Cr4+：YAG中没有光散射，则波长1300nm下的透射率包含因界面反射引起的损失在内应该达到约84％，因此，如果每1cm烧结体厚度的波长1300nm的光的透射率为80％以上，则判断为良好。
(Cr的价数评价)
从Cr3+向Cr4+的价数转变的评价使用X射线近边吸收光谱(XANES)并通过与作为参考试样的Cr3+：YAG烧结体进行比较来进行。需要说明的是，如前所述，在YAG中Cr与“Al原子”置换而存在，但是在YAG中Al原子具有在周围具有8个氧的八配位和在周围具有4个氧的四配位的状态。三价的Cr与八配位的Al原子进行置换，四价的Cr与四配位的Al原子进行置换。在对该Cr原子照射具有5980eV～6040eV的能量的X射线时，观测到Cr原子的K吸收边(从1s轨道向4p轨道的跃迁)。对该区域详细进行研究时，有时在5990eV附近出现独立的峰。这是伴随从1s轨道向3d轨道的跃迁的峰，原本是禁戒跃迁，但是通过利用晶体场形成3d轨道与4p轨道的杂化轨道而成为允许的跃迁，被称为边前峰(pre-edge peak)。对于以八配位存在的三价的Cr而言不出现该峰，对于以四配位存在的四价的Cr而言出现该峰。因此，通过测定该峰的强度，能够评价YAG中的四价Cr原子的转化率(Cr4+/(Cr3++Cr4+))。
(关于参考试样Cr3+：YAG)
以分别为34.48摩尔％、62.36摩尔％、0.06摩尔％、0.10摩尔％的方式称量Y2O3粉末、Al2O3粉末、Cr2O3粉末、Si(OC2H5)4。通过像这样不添加MgO粉末、CaCO3粉末而不进行价数补偿，Cr必然为三价。接着，与下述实施例1同样地由原料粉末制作浆料，然后添加Si(OC2H5)4和乳酸铝而制作造粒粉，然后进行成型、加热、烧制等，从而制作了参考试样用Cr3+：YAG烧结体。
(被动调Q的运行试验)
为了确认所制作的Cr4+：YAG是否发挥被动调Q的功能，利用图3中示出的装置进行试验。使来自产生808nm的激光的激光二极管13的光通过介质镜11(透射100％的808nm的光，反射100％的1064nm的光)，并入射至1原子％Nd：GdVO4晶体10。以夹着该晶体10的方式配置介质镜11和介质镜12(反射97％的1064nm的光)，在其前方配置检测1064nm的光的光检测器14。然后，利用介质镜11和介质镜12使从晶体10发射的1064nm的光折回而进行激光振荡。
[实施例]
以下，基于实施例和比较例进行说明。需要说明的是，本实施例仅是一个例子，不受该例任何制限。即，本发明仅受权利要求书限制，包含本发明所含的实施例以外的各种变形。
(实施例1)
如表1所示分别称量规定量的平均粒径为1μm的Y2O3粉末、Al2O3粉末、Cr2O3粉末、MgO粉末、CaCO3粉末作为原料，将这些原料粉末投入混合粉碎机中，利用以水为溶剂、以氧化铝为介质的球磨机进行5小时湿式混合，从而得到了浆料。
向该浆料中添加Si(OC2H5)4和乳酸铝并进行搅拌，然后使其干燥，然后通过喷雾干燥而得到了平均粒径为20μm～30μm的造粒粉。
接着，将该造粒粉放入模具(φ150mm×40mm)中并进行冷压，然后在176MPa下进行CIP成型。接着，在大气炉中将其在100℃下加热5小时，然后在900℃下加热2小时。
接着，在真空加热炉中对该成型体在1800℃下进行15小时烧制，然后在1700℃下、147MPa、Ar气氛中进行3小时的HIP。然后，在大气炉中、在1400℃下加热10小时，从而制作了φ150mm×40mm的Cr4+：YAG烧结体。
对通过以上步骤得到的烧结体进行成分分析，结果如表1所示，满足上述1)～3)的条件。对该烧结体测定波长1300nm的光的透射率，结果在厚度为1cm时显示出84％的优异的透光性。
接着，将对于实施例1的YAG烧结体和作为参考试样的Cr3+：YAG的K吸收边的XANES测定结果示于图1中。如图1所示，在实施例1中出现了位于5990eV附近的边前峰，但是在Cr3 +：YAG中未出现位于5990eV附近的边前峰。图2中示出进一步放大5990eV附近后的图。另外，在图2中一并示出了作为全部由四价Cr构成的晶体的铬酸四叔丁酯(Cr(Ot-Bu)4)的XANES测定光谱的结果。由于该铬酸四叔丁酯的峰强度为全部为四价Cr的情况下的强度，因此通过与铬酸四叔丁酯的峰强度的峰强度比而求出Cr4+/(Cr3++Cr4+)。由该强度比求出的值Cr4+/(Cr3++Cr4+)＝0.29。
接着，为了确认所制作的Cr：YAG是否发挥被动调Q的功能，使用图3中示出的装置进行了试验。将其结果示于图4中。图4的(31)为未插入Cr：YAG 20的状态的图，可知：无论何时，都检测到恒定的光强度信号。另一方面，图4的(32)～(35)示出将实施例1中制作的Cr：YAG 20插入Nd：GdVO4晶体10与介质镜12之间，改变来自激光二极管13的激发光强度，并改变振荡输出功率时的结果。如图4所示，光强度信号为脉冲形，观察到振荡输出功率越高，则脉冲周期越窄，确认发生了由Cr4+：YAG引起的被动调Q。图4的(36)示出此时的一个脉冲的形状。脉冲宽度为约80纳秒。
(实施例2～8)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。进行所得到的Cr：YAG烧结体的成分分析，结果如表1所示，均满足上述1)～3)的条件。另外，对各Cr：YAG烧结体与实施例1同样地测定波长1300nm的光的透射率，结果均在厚度为1cm时显示出80％以上的优异的透光性。此外，对该Cr：YAG烧结体与实施例1同样地利用XANES进行价数评价，结果转化率Cr4+/(Cr3++Cr4+)为至少0.25以上。另外，对于各Cr：YAG烧结体，使用图3中示出的装置进行与实施例1同样的试验，结果均确认到由被动调Q引起的脉冲振荡。
(比较例1)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述1)的条件。对该Cr：YAG烧结体测定波长1300nm的光的透射率，结果观察到在厚度为1cm时透光性降低为75％。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果激光振荡停止。认为这是由于透光性差，因此激光被遮蔽。
(比较例2)
除了如表1所述改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述2)的条件。对该Cr：YAG烧结体进行Cr的价数评价，结果为Cr4+/(Cr3++Cr4+)＝0.08。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果虽然发生激光振荡，但是未发生脉冲振荡，无论何时，都检测到恒定强度的光信号。这是因为Cr4+的浓度不足，未发生被动调Q。
(比较例3)
如表1所示改变原料粉末的称量比，另外，不添加Si(OC2H5)4，除此以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述3)的组成条件。对该Cr：YAG烧结体测定波长1300nm的光的透射率，结果观察到透光性降低为78％。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果激光振荡停止。认为这是由于透光性差，因此激光被遮蔽。
(比较例4)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述2)的条件。对该Cr：YAG烧结体进行Cr的价数评价，结果为Cr4+/(Cr3++Cr4+)＝0.01。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果虽然发生激光振荡，但是未发生脉冲振荡，无论何时，都检测到恒定强度的光信号。这是因为Cr4+的浓度不足，未发生被动调Q。
(比较例5)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述2)的条件。对该Cr：YAG烧结体进行Cr的价数评价，结果为Cr4+/(Cr3++Cr4+)＝0.01。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果虽然发生激光振荡，但是未发生脉冲振荡，无论何时，都检测到恒定强度的光信号。这是因为Cr4+的浓度不足，未发生被动调Q。
(比较例6)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述2)的条件。对该Cr：YAG烧结体进行Cr的价数评价，结果为Cr4+/(Cr3++Cr4+)＝0.10。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果虽然发生激光振荡，但是未发生脉冲振荡，无论何时，都检测到恒定强度的光信号。这是因为Cr4+的浓度不足，未发生被动调Q。
(比较例7)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述1)和2)的条件。对该Cr：YAG烧结体测定波长1300nm的光的透射率，结果观察到在厚度为1cm时透光性降低为60％。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果激光振荡停止。认为这是由于透光性差，因此激光被遮蔽。
(比较例8)
除了如表1所示改变原料粉末的称量比以外，通过与实施例1同样的方法制作了Cr：YAG烧结体。对该Cr：YAG烧结体进行成分分析，结果如表1所示，未满足上述2)的条件。对该Cr：YAG烧结体进行Cr的价数评价，结果为Cr4+/(Cr3++Cr4+)＝0.31。对该烧结体使用图3中示出的装置进行与实施例1同样的试验，结果虽然发生激光振荡，但是未发生脉冲振荡，无论何时，都检测到恒定强度的光信号。这是因为Cr4+的浓度不足，未发生被动调Q。
Figure BDA0002677535660000131
产业实用性
根据本发明，能够制造透光性优异并且Cr4+转化率高的Cr：YAG烧结体。本发明的实施方式的Cr：YAG烧结体可用于荧光体、激光介质等。
标号说明
10 1原子％Nd：GdVO4晶体
11 介质镜
12 介质镜
13 激光二极管
14 光检测器
20 Cr：YAG烧结体

Claims (3)

1.一种Cr：YAG烧结体，其特征在于，所述Cr：YAG烧结体含有Al、Y、Cr、Ca、Mg、Si和O，并且该烧结体中的成分含量满足下述1)～3)的条件式，其中，在条件式中，各元素符号表示成分含量(原子ppm)，
1)|(Y+Ca)/(Al+Cr+Si+Mg)-0.6|＜0.001，
2)0原子ppm≤(Ca+Mg)-(Cr+Si)≤50原子ppm，
3)50原子ppm≤Si≤500原子ppm。
2.如权利要求1所述的Cr：YAG烧结体，其特征在于，所述Cr：YAG烧结体的波长1300nm的光的透射率为80％以上。
3.如权利要求1或2所述的Cr：YAG烧结体，其特征在于，所述Cr：YAG烧结体的Cr4+的转化率为Cr4+/(Cr3++Cr4+)≥0.25。
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