CN105359236A - 层叠陶瓷电容器 - Google Patents

层叠陶瓷电容器 Download PDF

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CN105359236A
CN105359236A CN201480037368.3A CN201480037368A CN105359236A CN 105359236 A CN105359236 A CN 105359236A CN 201480037368 A CN201480037368 A CN 201480037368A CN 105359236 A CN105359236 A CN 105359236A
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ceramic
molar part
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mole
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CN105359236B (zh
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冈本贵史
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Murata Manufacturing Co Ltd
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Abstract

本发明提供一种高温负荷时的绝缘劣化耐性高的层叠陶瓷电容器。内层用陶瓷层(11)的组成是以含有Ba及Ti的钙钛矿型化合物作为主成分，含有Nb及Ta的至少一种，并且含有Mn及Al，并且任选地含有Mg及稀土类元素(Y、Gd、Tb、Dy、Ho、Er中的至少一种)，在将Ti的含量设为100摩尔份时，含有：(a)Nb及Ta的合计为0.2～1.5摩尔份、(b)Mg为0.2摩尔份以下(包括0摩尔份)、(c)Mn为1.0～3.5摩尔份、(d)Al为1.0～4.0摩尔份、(e)稀土类元素为0.05摩尔份以下(包括0摩尔份)。此外，每1层的内层用陶瓷层(11)的平均粒子数为3个以下。

Description

层叠陶瓷电容器
技术领域
本发明涉及一种层叠陶瓷电容器。
背景技术
以往，作为即使在低氧分压下烧成也不会半导体化、而且静电电容的温度特性平坦的层叠电容器用电介质材料，例如已经提出过很多以BaTiO3作为主成分的电介质陶瓷组合物。
而且，由于近年来的电子技术的发展，电子机器的高功能化及高集成化不断推进，层叠陶瓷电容器的使用条件变得越来越严苛。
特别是，由于电子机器的高集成化，安装在以高频动作的CPU等发热体的附近的层叠陶瓷电容器的周边温度与以往相比越来越高，有可能对可靠性造成影响。
另一方面，为了满足如前所述的层叠陶瓷电容器的小型大容量化的要求，还产生了将电介质陶瓷层进一步薄层化、并且多层化的需求。
在此种状况中，对于层叠陶瓷电容器，要求兼顾小型大容量化和绝缘耐力的提高。因而，作为用于该层叠陶瓷电容器所使用的电介质陶瓷组合物，需要如下的电介质陶瓷组合物：其介电常数高，且介电常数的温度特性平坦，即使将电介质陶瓷层薄层化，绝缘耐力和可靠性也优异。
例如，在专利文献1中，为了解决上述的要求，提出了一种电介质陶瓷组合物，是以组成式：100(Ba1-xCax)mTiO3+aMnO+bNb2O5+cSiO2+dRe2O3(其中，Re是选自Y、Eu、Gd、Tb、Dy、Ho、Er、Tm、以及Yb中的至少1种金属元素，a、b、c、以及d表示摩尔比)表示的电介质陶瓷组合物，处于0.01≤a≤5、0.05≤b≤2、0.4≤c≤8、0.05≤d≤2.5、0.01≤x≤0.20、0.99≤m≤1.03的范围内。
现有技术文献
专利文献
专利文献1：日本特开2005-132645号公报
发明内容
发明所要解决的问题
然而，使用了专利文献1的电介质陶瓷组合物的层叠陶瓷电容器的高温负荷时的绝缘电阻的经时变化大，存在有可靠性不够充分的不佳状况。
因而，本发明的目的在于，提供一种高温负荷时的绝缘劣化耐性高的层叠陶瓷电容器。
用于解决问题的方法
本发明提供一种层叠陶瓷电容器，其具备：层叠体，具有多个电介质陶瓷层、和沿着电介质陶瓷层间的界面形成的多个内部电极；和多个外部电极，形成于层叠体的外表面，且与内部电极电连接；其中，电介质陶瓷层的组成是以含有Ba及Ti的钙钛矿型化合物作为主成分，含有Nb及Ta的至少一种，并且含有Mn及Al，并且任选地含有Mg及稀土类元素，稀土类元素(Y、Gd、Tb、Dy、Ho、Er中的至少一种)，在将Ti的含量设为100摩尔份时，含有：(a)Nb及Ta的合计为0.2～1.5摩尔份、(b)Mg为0.2摩尔份以下(包括0摩尔份)、(c)Mn为1.0～3.5摩尔份、(d)Al为1.0～4.0摩尔份、(e)稀土类元素为0.05摩尔份以下(包括0摩尔份)，每1层的电介质陶瓷层的平均粒子数为3个以下。需要说明的是，所谓“每1层的电介质陶瓷层的平均粒子数”是指沿着1个电介质陶瓷层的厚度方向存在的陶瓷粒子(陶瓷晶界)的平均个数。
本发明中，电介质陶瓷层所含的稀土类元素为0.05摩尔份以下(包括0摩尔份)，因此成为高温负荷时的绝缘劣化耐性优异的层叠陶瓷电容器。此外，由于每1层的电介质陶瓷层的平均粒子数(平均晶界数)少到3个以下，因此由于晶界的原因而产生的故障减少，可以实现更高的绝缘劣化耐性。
因而，电介质陶瓷层中所含的稀土类元素为0.05摩尔份以下(包括0摩尔份)、与每1层的电介质陶瓷层的平均粒子数(平均晶界数)为3个以下协同地作用而可以得到显著的绝缘劣化耐性。
发明效果
根据本发明，可以得到高温负荷时的绝缘劣化耐性优异的层叠陶瓷电容器。
本发明的上述目的、其他目的、特征及优点将会由参照附图进行的用于实施以下的发明的方式的说明而更加明确。
附图说明
图1是表示本发明的层叠陶瓷电容器的一个实施方式的剖面图。
具体实施方式
将本发明的层叠陶瓷电容器的一个实施方式与其制造方法一起进行说明。
1.层叠陶瓷电容器
图1是表示层叠陶瓷电容器1的长度(L)方向的垂直剖面图。层叠陶瓷电容器1具备陶瓷主体10、和形成于陶瓷主体10的左右的端部的外部电极20、22。
陶瓷主体10具有长方体形状的层叠体结构，该层叠体结构由多个内层用陶瓷层11、配设于多个内层用陶瓷层11彼此的界面处的多个内部电极12、13、配设于上下而夹持多个内层用陶瓷层11的外层用陶瓷层15a、15b构成。
内部电极12与内部电极13在厚度方向上隔着内层用陶瓷层11而对置。该内部电极12和内部电极13在隔着内层用陶瓷层11而对置的部分形成了静电电容。
内部电极12的左侧端部被引出至陶瓷主体10的左侧的端面而与外部电极20电连接。内部电极13的右侧端部被引出至陶瓷主体10的右侧的端面而与外部电极22电连接。
内层用陶瓷层11由电介质陶瓷组合物构成。配设于上下的外层用陶瓷层15a、15b也分别使用与内层用陶瓷层11相同的电介质陶瓷组合物。需要说明的是，外层用陶瓷层15a、15b也可以由与内层用陶瓷层11不同的电介质陶瓷组合物构成。
关于内层用陶瓷层11的组成，以含有Ba及Ti的钙钛矿型化合物作为主成分，含有Nb及Ta的至少一种，并且含有Mn及Al，并且任选地含有Mg及稀土类元素(Y、Gd、Tb、Dy、Ho、Er中的至少一种)，在将Ti的含量设为100摩尔份时，含有：
(a)Nb及Ta的合计为0.2～1.5摩尔份、
(b)Mg为0.2摩尔份以下(包括0摩尔份)、
(c)Mn为1.0～3.5摩尔份、
(d)Al为1.0～4.0摩尔份、
(e)稀土类元素为0.05摩尔份以下(包括0摩尔份)。
此外，每1层的内层用陶瓷层11的平均粒子数为3个以下。所谓“每1层的内层用陶瓷层11的平均粒子数”是指沿着1个内层用陶瓷层11的厚度方向所存在的陶瓷粒子(陶瓷晶界)的平均个数。
关于具有以上构成的层叠陶瓷电容器1，由于内层用陶瓷层11所含的稀土类元素为0.05摩尔份以下(包括0摩尔份)，因此成为高温负荷时的绝缘劣化耐性优异的层叠陶瓷电容器。此外，由于每1层的内层用陶瓷层11的平均粒子数(平均晶界数)少到3个以下，因此由于晶界的原因而产生的故障减少，可以实现更高的绝缘劣化耐性。
因而，内层用陶瓷层11所含的稀土类元素为0.05摩尔份以下(包括0摩尔份)与每1层的内层用陶瓷层11的平均粒子数(平均晶界数)为3个以下协同地作用，发挥出可以获得显著的绝缘劣化耐性的协同效应。
2.层叠陶瓷电容器的制造方法
下面，对层叠陶瓷电容器1的制造方法进行说明。
首先，称量准备出用于电介质陶瓷组合物的原料粉末。用于电介质陶瓷组合物的原料粉末以含有Ba及Ti的钙钛矿型化合物作为主成分。此外，作为副成分，含有Nb及Ta中的至少一种，并且含有Mn及Al，并且任选地含有Mg及稀土类元素(Y、Gd、Tb、Dy、Ho、Er中的至少一种)，在将Ti的含量设为100摩尔份时，含有：
(a)Nb及Ta的合计为0.2～1.5摩尔份、
(b)Mg为0.2摩尔份以下(包括0摩尔份)、
(c)Mn为1.0～3.5摩尔份、
(d)Al为1.0～4.0摩尔份、
(e)稀土类元素为0.05摩尔份以下(包括0摩尔份)。
该电介质陶瓷组合物是非还原性电介质材料，即使在还原性气氛中进行烧成，也可以烧结而不发生半导体化。
之后，用于电介质陶瓷组合物的原料粉末被浆料化。该浆料被成形为片状，得到用于内层用陶瓷层11及外层用陶瓷层15a、15b的陶瓷生片。
然后，在用于内层用陶瓷层11的陶瓷生片的表面，形成内部电极12、13。内部电极12、13由选自Ni、Ni合金、Cu及Cu合金中的至少1种导电性材料构成。内部电极12、13是使用由导电性材料构成的导电性糊剂、并利用丝网印刷法或转印法等形成的。
然后，将形成了内部电极12、13的用于内层用陶瓷层11的陶瓷生片层叠所需的数目后，使这些陶瓷生片被用于外层用陶瓷层15a、15b的陶瓷生片夹持，制成层叠体。通过对层叠体进行热压接，而制成未烧成的层叠体。
然后，将未烧成的层叠体在规定的还原性气氛中以规定的温度烧成，制成如图1所示的烧结了的陶瓷主体10。
之后，在陶瓷主体10的两个端部，分别形成外部电极20、22。外部电极20、22分别与内部电极12、13电连接。作为外部电极20、22的材料，可使用Ni、Ni合金、Cu、Cu合金、Ag、或Ag合金等。外部电极20、22通过如下方式形成：将向金属粉末中添加玻璃料而得的导电性糊剂涂布在陶瓷主体10的两端部并烧接。
需要说明的是，将成为外部电极20、22的导电性糊剂也可以涂布于未烧成的陶瓷主体10，并在陶瓷主体10的烧成的同时被烧接。另外，根据需要，也可以在外部电极20、22上，形成Ni、Cu、焊料、Sn等的镀层。
根据以上的方法，可以可靠地批量生产高温负荷时的绝缘劣化耐性优异的层叠陶瓷电容器1。
实施例
1.实施例及比较例
制作实施例及比较例的试样(层叠陶瓷电容器1)，进行每1层的内层用陶瓷层11的平均粒子数测定及高温负荷寿命试验。
(电介质陶瓷组合物的制作)
对于作为主成分的钛酸钡的起始原料而言，准备了BaCO3粉末及TiO2粉末。称量各材料，从而在将Ti的含量设为100摩尔份时，使Ba的含量为104摩尔份，以水作为介质利用球磨机混合。之后，在1050℃煅烧，将所得的煅烧粉末粉碎，得到主成分的钛酸钡粉末。需要说明的是，也可以在该钛酸钡的Ba位点含有Ca、Sr，在Ti位点含有Zr、Hf。
然后，在该主成分的钛酸钡粉末中，作为添加成分，添加了Nb2O5、Ta2O5、Dy2O3、Al2O3、MgCO3、MnCO3，从而在将主成分的Ti的含量设为100摩尔份时，使各副成分的量为表1所示的组成(记为mol份)。此外，作为烧结助剂，相对于Ti的含量100摩尔份而加入4.0摩尔份的SiO3，利用球磨机在水中混合，得到电介质陶瓷组合物粉末。
对所得的电介质陶瓷组合物粉末，利用ICP发光分光分析确认，与表1所示的组成几乎相同。
(陶瓷生片的制作)
向该电介质陶瓷组合物粉末中，加入聚乙烯醇缩丁醛系粘合剂及乙醇等有机溶媒，利用球磨机进行湿式混合，制作出陶瓷浆料。将该陶瓷浆料利用刮刀法成形出用于内层用陶瓷层11的陶瓷生片，而使烧成后的内层用陶瓷层11的厚度为3.0μm。同样地，成形出规定的厚度的用于外层用陶瓷层15a、15b的陶瓷生片。
(层叠陶瓷电容器的制作)
然后，在用于内层用陶瓷层11的陶瓷生片上，丝网印刷含有Ni作为导电成分的导电性糊剂，形成内部电极12、13。
然后，将形成有内部电极12、13的陶瓷生片层叠多片，使内部电极12、13的引出部交错。之后，将这些形成有内部电极12、13的陶瓷生片以用于外层用陶瓷层15a、15b的陶瓷生片夹持，制成层叠体结构的未烧成的陶瓷主体10。
然后，将该未烧成的陶瓷主体10在空气气氛中加热到270℃，使粘合剂燃烧。之后，将陶瓷主体10在由H2-N2-H2O气体构成的PO2＝10-9～-10.5(atm)的还原性气氛中，在1140～1220℃(表1中示出各试样的烧成温度)的烧成温度保持2小时，得到致密的烧结陶瓷主体10。
对所得的陶瓷主体10利用ICP发光分光分析确认，除了内部电极12、13的Ni成分以外，与表1中所示的组成大致上相同。
然后，在烧结了的陶瓷主体10的两个端面，烧接Cu的外部电极20、22，制成试样的层叠陶瓷电容器1。
所得的层叠陶瓷电容器1的外形尺寸是：宽度(W)为1.0mm、长度(L)为2.0mm、厚度(T)为0.7mm。介于内部电极12、13间的内层用陶瓷层11的厚度为3.0μm，内部电极12、13的厚度为1.0μm。另外，有效内层用陶瓷层11的总数为160，每一层的对置电极面积为1.6mm2。
2.实施例及比较例的评价方法
(内层用陶瓷层的每1层的平均粒子数测定)
每1层的内层用陶瓷层11的平均粒子数是利用截距法求出。
具体而言，将层叠陶瓷电容器1的长度(L)方向的约1/2的位置截断，制作露出了WT剖面的试样。之后，为了使露出于WT剖面的陶瓷的晶粒间的边界(晶界)清楚，对试样进行了热处理。热处理的温度是晶粒不会生长的温度、且设为使晶界清楚的温度，本实施例为1000℃。
在WT剖面的宽度(W)方向及厚度(T)方向的各自约1/2的位置处，利用扫描型电子显微镜(SEM)以10，000倍观察内层用陶瓷层11的晶粒。在所得的SEM图像中，以2μm以上的间隔随机地引出100条与内部电极12、13正交的线。1条线的长度必然大致上是内层用陶瓷层11的1层的厚度(3.0μm)。此后，将各条线所横切的陶瓷粒子的数的合计除以100，将所得的值设为每1层的内层用陶瓷层11的平均粒子数。
(高温负荷寿命试验)
关于高温负荷寿命试验，是在170℃的温度的环境下，在施加30V/3μm(3μm为内层用陶瓷层11的1层的厚度)的电压的状态下，测定出层叠陶瓷电容器1的绝缘电阻的经时变化。而且，当绝缘电阻值为50kΩ以下时，则判定为故障，根据故障时间的威布尔分析求出50％的平均故障时间(MTTF)。而且，在MTTF短于150小时的情况下，认为不合格。试样数为100。
(介电常数测定)
内层用陶瓷层11的介电常数是根据层叠陶瓷电容器1的静电电容算出的。
3.实施例及比较例的特性评价结果
表1示出每1层的内层用陶瓷层11的平均粒子数测定及高温负荷寿命试验的评价结果。带有※标记的试样编号的层叠陶瓷电容器1属于本发明的范围外。
[表1]
※本发明的范围外
根据表1可以确认，在属于本发明的范围内的试样编号3、5、7、10、12、16、18、22、24、27、29、31、34、37、40的层叠陶瓷电容器1的情况下，具有优异的高温负荷寿命。另外，还确认具有高介电常数。
这些试样编号3、5、7……的层叠陶瓷电容器1的内层用陶瓷层11的组成是以钛酸钡作为主成分，含有Nb及Ta的至少一种，并且含有Mn及Al，并且任选地含有Mg及稀土类元素(Y、Gd、Dy、Er中的至少一种)，在将Ti的含量设为100摩尔份时，含有：
(a)Nb及Ta的合计为0.2～1.5摩尔份、
(b)Mg为0.2摩尔份以下(包括0)、
(c)Mn为1.0～3.5摩尔份、
(d)Al为1.0～4.0摩尔份、
(e)稀土类元素为0.05摩尔份以下(包括0)，
每1层的内层用陶瓷层11的平均粒子数为3个以下。
此种情况下，高温负荷时的绝缘劣化耐性与以往的稀土类组成(像专利文献1那样，稀土类元素多到0.1摩尔份以上的组成)的情况相比变得优良。即，如果含有一定量以上的稀土类元素，则在每1层的内层用陶瓷层11的平均粒子数降低的情况下，难以维持高温负荷时的绝缘电阻。
另一方面，在属于本发明的范围外的试样编号1、8的层叠陶瓷电容器1的情况下(内层用陶瓷层11的Nb的添加量过少、或过多的情况下)，即使每1层的内层用陶瓷层11的平均粒子数为3个以下，高温负荷时的绝缘电阻也明显地劣化。
在属于本发明的范围外的试样编号2、4、6、9、11、15、17、21、23、26、28、30、33、36、39的层叠陶瓷电容器1的情况下(即使内层用陶瓷层11的Nb、Ta等的添加量合适，然而每1层的内层用陶瓷层11的平均粒子数多于3个的情况下)，虽然高温负荷时的绝缘电阻没有明显劣化，然而属于标准外。
在属于本发明的范围外的试样编号13的层叠陶瓷电容器1的情况下(即使内层用陶瓷层11的Nb、Ta的添加量合适，然而Mg添加量大于0.2摩尔份的情况下)，即使每1层的内层用陶瓷层11的平均粒子数为3个以下，高温负荷时的绝缘电阻也发生了劣化。
在属于本发明的范围外的试样编号14、19的层叠陶瓷电容器1的情况下(内层用陶瓷层11的Al的添加量为1.0～4.0摩尔份的范围外的情况下)，即使每1层的内层用陶瓷层11的平均粒子数为3个以下，高温负荷时的绝缘电阻也发生了劣化。
在属于本发明的范围外的试样编号20、25的层叠陶瓷电容器1的情况下(内层用陶瓷层11的Mn的添加量为1.0～3.5摩尔份的范围外的情况下)，即使每1层的内层用陶瓷层11的平均粒子数为3个以下，高温负荷时的绝缘电阻也发生了劣化。
在属于本发明的范围外的试样编号32、35、38、41的层叠陶瓷电容器1的情况下(内层用陶瓷层11的稀土类元素(Dy、Gd、Er、Y)的添加量大于0.05摩尔份的情况下)，即使每1层的内层用陶瓷层11的平均粒子数为3个以下，平均故障时间(MTTF)也小。
需要说明的是，本发明并不限定于所述实施方式，可以在其主旨的范围内进行各种变形。
符号的说明
1层叠陶瓷电容器
10陶瓷主体
11内层用陶瓷层
12、13内部电极
15a、15b外层用陶瓷层
20、22外部电极

Claims (1)

1.一种层叠陶瓷电容器，其具备：
层叠体，具有多个电介质陶瓷层、和沿着所述电介质陶瓷层间的界面形成的多个内部电极；和
多个外部电极，形成于所述层叠体的外表面，且与所述内部电极电连接；其中，
所述电介质陶瓷层的组成是以含有Ba及Ti的钙钛矿型化合物作为主成分，含有Nb及Ta的至少一种，并且含有Mn及Al，并且任选地含有Mg及稀土类元素，所述稀土类元素为Y、Gd、Tb、Dy、Ho、Er中的至少一种，在将Ti的含量设为100摩尔份时，含有：
(a)Nb及Ta的合计为0.2～1.5摩尔份，
(b)Mg为0.2摩尔份以下且包括0摩尔份，
(c)Mn为1.0～3.5摩尔份，
(d)Al为1.0～4.0摩尔份，
(e)稀土类元素为0.05摩尔份以下且包括0摩尔份，
每1层的所述电介质陶瓷层的平均粒子数为3个以下。
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