CN102531591A - 具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和多层陶瓷电容器的制备方法 - Google Patents

具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和多层陶瓷电容器的制备方法 Download PDF

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Publication number
CN102531591A
CN102531591A CN2011103501662A CN201110350166A CN102531591A CN 102531591 A CN102531591 A CN 102531591A CN 2011103501662 A CN2011103501662 A CN 2011103501662A CN 201110350166 A CN201110350166 A CN 201110350166A CN 102531591 A CN102531591 A CN 102531591A
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accessory constituent
dielectric combination
dielectric
mole
under
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姜晟馨
宋旻星
崔斗源
权祥勋
金昶勋
许康宪
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Samsung Electro Mechanics Co Ltd
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Samsung Electro Mechanics Co Ltd
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Priority claimed from KR1020110081718A external-priority patent/KR20120089549A/ko
Application filed by Samsung Electro Mechanics Co Ltd filed Critical Samsung Electro Mechanics Co Ltd
Publication of CN102531591A publication Critical patent/CN102531591A/zh
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Abstract

本发明公开了具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和多层陶瓷电容器的制备方法。该介电组合物包括：作为主要组分的由通式(Ba1-xCax)m(Ti1-yZry)O3(0.995≤m≤1.010，0.001≤x≤0.10，0.001≤y≤0.20)表示的化合物；作为第一次要组分的铝氧化物；作为第二次要组分的选自由Mg、Sr、Ba、Ca、和Zr组成的组中的至少一种金属及其盐；作为第三次要组分的选自由Sc、Y、La、Ac、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、和Lu组成的组中的至少一种金属及其盐；作为第四次要组分的选自由Cr、Mo、W、Mn、Fe、Co、和Ni组成的组中的至少一种金属及其盐；以及选自含有Si的玻璃形成化合物的第五次要组分。该介电组合物满足在EIA规范中定义的Y5V或X5R特性。

Description

具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和多层陶瓷电容器的制备方法
相关申请的引用
本申请要求于2010年11月8日和2011年8月17日提交的题为“Dielectric Composition Having High Dielectric Constant，Multi LayeredCeramic Condensers Comprising the Same，and Method of Preparing for MultiLayered Ceramic Condensers(具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和多层陶瓷电容器的制备方法)”的韩国专利申请系列号10-2010-0110368和10-2011-0081718的权益，由此将其全部内容通过引用并入本申请中。
技术领域
本发明涉及一种具有高介电常数的介电组合物(电介质组合物，dielectric composition)、包括其的多层陶瓷电容器、和用于多层陶瓷电容器的制备方法，更具体地，涉及一种具有高介电常数的满足在EIA规范中定义的Y5V特性的介电组合物、包括其的MLCC、和用于多层陶瓷电容器的制备方法。
背景技术
根据相关领域的多层陶瓷电容器已通过重复将包含基于钛酸钡的粉末作为主要组分和用于调节特性的金属氧化物作为次要组分的陶瓷介电材料模制成片状以制备生片(green sheet)并将印刷电极层叠在生片上的工艺而制备。
在最近的电子和电气工业中，高集成、微型化和轻巧已快速发展。因此，对于具有高电容(容量)和小尺寸并具有耐热性、可靠性等的陶瓷电容器存在需求。
多层陶瓷电容器根据电容的温度特性系数(TCC)分为诸如Y5V(在-50℃至85℃下±15％至-82％)、X5R(在-55℃至85℃下在±15％以内)、X7R(在-55℃至125℃下±15％)的产品。在将介电层微减薄至3μm或更小的情况下，目前通常使用具有X5R特性的产品。
同时，虽然贵金属如Pd、Ag等已经被用作多层陶瓷电容器的内部电极，但目前使用具有低成本的贱金属如Ni等。在使用诸如Ni的贱金属作为内部电极的情况下，由于电极在烧制过程中被氧化，因此应当在还原气氛下对其进行烧制。然而，当电极在还原气氛下烧制时，介电层被还原，使得比电阻变小。因此，已经开发了甚至在还原气氛下不会被还原的非还原性介电材料。
在日本专利特许公开第20000-311828号中提出的利用介电磁性组合物的多层陶瓷电容器在直流电场下具有低的电容的老化变化和低的电容的劣化。然而，介电磁性组合物应该在1270℃或更高的高温下烧制。另外，当在多层陶瓷电容器中具有3μm厚度的电介质层叠为四层时，使介电磁性组合物实现具有8085或更低的介电常数。因此，介电磁性组合物可能不会实现将多层陶瓷电容器的介电层减薄至2μm的水平以及具有低的介电常数。
通常，当烧制温度高于1250℃时，诸如Ni的贱金属的内部电极层比介电层收缩更快，从而在两层之间引起分层现象。另外，由于内部电极的熔结现象引起的短路缺陷的可能性增加，并且当减薄介电层时短路缺陷的可能性进一步增加。
即，根据相关领域的介电组合物需要在1250℃或更高的高温下烧制，即强烈的还原烧制。因此，因为由于强烈的还原烧制引起的如电极熔结等的问题，在芯片内经常会产生裂纹。因此，迫切地需要能够在低温和弱还原条件下进行烧制的组合物。
发明内容
本发明的一个目的是提供一种满足在EIA规范中定义的Y5V或X5R特性的介电组合物。
本发明的另一个目的是提供包含具有高介电常数的介电组合物的多层陶瓷电容器。
本发明的另一个目的是提供一种能够在低温和弱还原气氛下进行烧制的多层陶瓷电容器的制备方法。
根据本发明的示例性实施方式，提供了一种具有高介电常数的介电组合物，包括：作为主要组分的由通式(Ba1-xCax)m(Ti1-yZry)O3(0.995≤m≤1.010，0.001≤x≤0.10，0.001≤y≤0.20)表示的化合物；作为第一次要组分的铝氧化物；作为第二次要组分的选自由Mg、Sr、Ba、Ca、和Zr组成的组中的至少一种金属及其盐；作为第三次要组分的选自由Sc、Y、La、Ac、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、和Lu组成的组中的至少一种金属及其盐；作为第四次要组分的选自由Cr、Mo、W、Mn、Fe、Co、和Ni组成的组中的至少一种金属及其盐；以及选自含有Si的玻璃形成化合物的第五次要组分。
介电组合物可以包含基于100摩尔主要组分为0.001至1.0摩尔的第一次要组分、0.01至4.00摩尔的第二次要组分、0.01至3.0摩尔的第三次要组分、0.01至1.5摩尔的第四次要组分、以及0.3至3.5摩尔的第五次要组分。
介电组合物可以满足在EIA规范中定义的Y5V或X5R特性。
根据本发明的另一个示例性实施方式，提供了包含具有高介电常数的介电组合物的多层陶瓷电容器。
根据本发明的另一个示例性实施方式，提供了一种用于多层陶瓷电容器的制备方法，包括：混合包含主要组分和次要组分的原料粉末(未加工粉末，粗粉末)以制备介电组合物；模制和层叠介电组合物以制备多层陶瓷片；以及增塑多层陶瓷片，然后在还原气氛下对多层陶瓷片进行烧制和再氧化。
还原气氛可以为0.01％至1.0％的H2。
烧制多层陶瓷片可以在1150℃至1250℃的温度下进行。
具体实施方式
在下文中，将详细地描述本发明。
本说明书中所使用的术语是为了解释实施方式而不是限制本发明。除非明确相反地描述，否则在本说明书中单数形式包括复数形式。词语“包括”以及变体如“包含”或“含有”将理解为是指包括规定的组分、步骤、操作和/或要素(元素)但不排除任何其他的组分、步骤、操作和/或要素(元素)。
本发明涉及具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和用于多层陶瓷电容器的制备方法。
根据本发明的示例性实施方式的介电组合物可以包括作为主要组分的由通式(Ba1-xCax)m(Ti1-yZry)O3(0.995≤m≤1.010，0.001≤x≤0.10，0.001≤y≤0.20)表示的化合物；作为第一次要组分的铝氧化物；作为第二次要组分的选自由Mg、Sr、Ba、Ca、和Zr组成的组中的至少一种金属及其盐；作为第三次要组分的选自由Sc、Y、La、Ac、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、和Lu组成的组中的至少一种金属及其盐；作为第四次要组分的选自由Cr、Mo、W、Mn、Fe、Co、和Ni组成的组中的至少一种金属及其盐；以及选自含有Si的玻璃形成化合物的第五次要组分。
根据本发明的示例性实施方式的介电组合物的主要组分通过在BaTiO3中用Ca取代一部分Ba并且用Zr取代一部分Ti而形成。在本发明的主要组分中，将Ca取代进入BaTiO3中以形成部分氧空位，由此提供耐还原性。因此，虽然在烧制后没有形成或很少地(thinly)形成核-壳结构，但是介电组合物可以表现出高绝缘电阻。取代的Ca的量为0.001≤x≤0.1摩尔。当x值超过0.1摩尔时，温度特性提高；然而，会出现常温介电常数劣化的问题。
另外，用Zr取代一部分Ti以使相变温度移至约85℃，由此实现Y5V特性并提高常温介电常数。y的含量为0.001≤y≤0.20摩尔，当y值超过0.20摩尔时，常温介电常数增加；然而，会出现温度特性劣化的问题。
另外，在由(Ba1-xCax)m(Ti1-yZry)O3表示的主要组分中，基于1的(Ti1-yZry)，(Ba1-xCax)优选在0.995≤m≤1.010的范围内。当m值低于0.995时，介电组合物在还原气氛下的烧制中容易被还原从而易于变成半导体材料，并且当其超过1.010时，会出现烧制温度过度升高并且可能不会实现期望的温度特性的问题。
同时，根据本发明的示例性实施方式的介电组合物可以通过在主要组分中包含多种次要组分来制备。具体地，介电组合物可以包括基于100摩尔主要组分为0.001至1.0摩尔的第一次要组分、0.01至4.00摩尔的第二次要组分、0.01至3.0摩尔的第三次要组分、0.01至1.5摩尔的第四次要组分、和0.3至3.5摩尔的第五次要组分。
根据本发明的示例性实施方式，可以加入作为铝氧化物的第一次要组分以便降低介电组合物中的烧制温度，并且基于100摩尔的主要组分，使第一次要组分在0.001至1.0摩尔的范围内被包括在介电组合物中。
当第一次要组分的含量低于0.001摩尔时，介电组合物可能不会在期望的温度下被烧制，并且当其超过1.0摩尔时，难于实现介电组合物的期望的介电常数。
另外，根据本发明的示例性实施方式的介电组合物可以包括作为第二次要组分的选自由Mg、Sr、Ba、Ca、和Zr组成的组中的至少一种金属及其盐。在介电组合物中优选包含基于100摩尔的主要组分为0.01至4.00摩尔的第二次要组分。当第二次要组分的含量低于0.01摩尔或超过4.00摩尔时，出现可能不会获得高的介电常数的问题。
另外，根据本发明的示例性实施方式的介电组合物可以包括作为第三次要组分的选自由Sc、Y、La、Ac、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、和Lu组成的组中的至少一种金属及其盐。
基于100摩尔的主要组分，在介电组合物中优选包括0.01至3.0摩尔的第三次要组分。当第三次要组分的含量低于0.01摩尔时，会出现高温加速寿命(high-temperature accelerated life)不能达到期望的水平的问题，而当其超过3.0摩尔时，会出现烧制温度升高以及可能不能获得期望的介电常数值的问题或出现由于第二相的产生引起的可靠性劣化问题。
另外，根据本发明的示例性实施方式的介电组合物可以包含作为第四次要组分的选自由Cr、Mo、W、Mn、Fe、Co、和Ni组成的组中的至少一种金属及其盐。
基于100摩尔的主要组分，在介电组合物中优选包含0.01至1.5摩尔的第四次要组分。当第四次要组分的含量低于0.01摩尔时，会出现高温加速寿命不能达到期望的水平的问题，而当其超过1.5摩尔时，会出现C*R值下降(即，这意味着数值下降，使得作为电容器的值劣化)以及电容随时间的变化变大的问题。
在第二至第四次要组分中包括的金属的盐没有特别限制。例如，选自由氧化物、碳酸盐、氯化物、醋酸盐、醇盐、和氮化物组成的组中的一种或多种物质可以用作包括在第二至第四次要组分中的金属的盐。
另外，根据本发明的示例性实施方式的介电组合物可以包含选自含有Si的玻璃形成化合物的第五次要组分。第五次要组分没有特别限制，只要其是能够与玻璃组合物中的其他组分结合以形成玻璃的化合物。例如，含有Si的氧化物、含有Si的玻璃化合物等可以用作第五次要组分。
基于100摩尔的主要组分，在介电组合物中优选包含0.3至3.5摩尔的第五次要组分。当第五次要组分的含量低于0.3摩尔时，会出现烧制温度升高以及烧制窗口变窄的问题，而当其超过3.5摩尔时，烧制温度可能会降低且烧制窗口变宽；然而，可能不会实现足够的介电常数。
由根据本发明示例性实施方式的介电组合物制备的介电层在X5R特性的情况下具有2500或更高的高介电常数(ε)，而在Y5V特性的情况下具有7000或更高的高介电常数(ε)。
并且，介电组合物满足在EIA规范中定义的Y5V特性(在-50℃至85℃下±15％至-82％)或X5R特性(在-55℃至85℃下在±15％以内)两者。
即，介电组合物可以在比现有的Y5V更低的温度，例如，在1250℃或更低，更优选1220℃或更低以及更弱的还原气氛(1％或更低的H2)下进行烧制，从而使得可以解决由于高温或强烈的还原气氛产生的缺陷如裂纹等。
另外，本发明可以提供包含由具有高介电常数的介电组合物制备的介电层的多层陶瓷电容器。
根据本发明的用于多层陶瓷电容器的制备方法可以包括混合包含主要组分和次要组分的原料粉末以制备介电组合物；模制和层叠介电组合物以制备多层陶瓷片；以及增塑多层陶瓷片，然后在还原气氛下对多层陶瓷片进行烧制和再氧化。
在利用介电组合物制备陶瓷片的情况下，可以使用普通的粘合剂、溶剂等，无需特别限制于此。
尤其是，根据本发明的示例性实施方式，制备多层陶瓷电容器中的还原气氛可以在0.01～1.0％的H2条件下，其可以是比现有的强还原条件低得多的条件。因此，在该弱还原气氛下烧制多层陶瓷电容器的情况下，可以解决在强还原气氛下烧制多层陶瓷电容器中产生的许多缺陷问题。
另外，根据本发明的用于多层陶瓷电容器的制备方法，多层片的烧制可以在1150至1250℃的低温下进行。根据相关领域的多层片的烧制主要是仅在超过1250℃的高温下进行。因此，可能会出现如裂纹等的缺陷问题。然而，根据本发明的示例性实施方式，烧制温度降低，由此使得可以解决这些问题。
在下文中，将参考实施例对本发明进行详细地描述。提供本发明的实施例以便向本领域技术人员更完全地解释本发明。下面的实施例可以以许多不同的形式进行更改并且不限制本发明的范围。相反，提供这些实施例，以便使本发明公开内容更加彻底和完整并且将本发明的思想完全地传达给本领域技术人员。
实施例1至11和比较例1至12
利用氧化锆球作为混合/分散介质，将由如下面的表1中所示的组合物制成的原料粉末与乙醇/甲苯和分散剂以及粘合剂进行混合，然后球磨15小时。使用制备的浆料从而利用以小刮刀模式的涂布机来制备具有3至5μm的活性模制片和具有10至13μm厚度的盖模片(cover moldingsheet)。在对内部电极进行压印、增塑、在还原气氛(0.08％的H2)下在如下面的表1中在1100至1300℃的温度下烧制2小时，然后在1000℃下进行用于再氧化的热处理3小时以后，层叠活性模制片25层并且层叠盖模片(10至13μm的厚度)20层。
将Ni电极压印并堆叠在模制的陶瓷片上，增塑经压缩和切割的片用于脱粘合剂(de-binder)，然后在1150至1250℃的温度下进行烧制以获得多层陶瓷电容器。
表1
Figure BDA0000106486130000091
Figure BDA0000106486130000101
实验例
利用LCR计在1kHz和1V下测量常温下的电容和介电损耗，并且在施加DC 250V的状态下在60秒后测量常温下的绝缘性。电容随温度的变化在-55℃至85℃的范围内进行测量。其结果在表2中示出。
表2
Figure BDA0000106486130000111
如在表1和2中可以了解到，当使用根据本发明示例性实施方式的电介质组分时，其可以在低温和弱还原气氛下烧制。另外，可以了解到，在根据本发明示例性实施方式的介电组合物的情况中，所有制备的介电层的介电常数高于使用偏离本发明范围的介电组合物的比较例。
并且，根据本发明示例性实施方式的介电组合物已经满足在EIA规范中定义的Y5V特性(在-50℃至85℃下±15％至-82％)和X5R特性(在-55℃至85℃下在±15％以内)两者。
如上面所阐述的，根据本发明的示例性实施方式，介电磁性组合物可以在1250℃或更低的低温和弱还原气氛(1％或更低的H2)下烧制，由此使得可以解决由于强还原气氛和高温产生的如裂纹等的缺陷。
因此，根据本发明示例性实施方式的介电磁性组合物可以用于各种电介质产品，例如，MLCC、压电元件、片式电感器、片式变阻器(chipvaristor)、片式电阻器等。
尤其是，根据本发明示例性实施方式的介电磁性组合物具有满足在EIA规范中定义的Y5V或X5R特性的高介电常数。
虽然已经结合示例性实施方式示出和描述了本发明，但对于本领域技术人员来说显而易见的是，在不背离如由所附权利要求所限定的本发明的精神和范围的情况下，可以进行更改和变化。

Claims (7)

1.一种具有高介电常数的介电组合物，包括：
作为主要组分的由通式(Ba1-xCax)m(Ti1-yZry)O3表示的化合物，0.995≤m≤1.010，0.001≤x≤0.10，0.001≤y≤0.20；
作为第一次要组分的铝氧化物；
作为第二次要组分的选自由Mg、Sr、Ba、Ca、和Zr组成的组中的至少一种金属及其盐；
作为第三次要组分的选自由Sc、Y、La、Ac、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、和Lu组成的组中的至少一种金属及其盐；
作为第四次要组分的选自由Cr、Mo、W、Mn、Fe、Co、和Ni组成的组中的至少一种金属及其盐；以及
选自含有Si的玻璃形成化合物的第五次要组分。
2.根据权利要求1所述的具有高介电常数的介电组合物，其中，所述介电组合物包含基于100摩尔的所述主要组分为0.001至1.0摩尔的所述第一次要组分、0.01至4.00摩尔的所述第二次要组分、0.01至3.0摩尔的所述第三次要组分、0.01至1.5摩尔的所述第四次要组分、和0.3至3.5摩尔的所述第五次要组分。
3.根据权利要求1所述的具有高介电常数的介电组合物，其中，所述介电组合物满足在EIA规范中定义的Y5V或X5R特性。
4.多层陶瓷电容器，包括根据权利要求1所述的具有高介电常数的介电组合物。
5.一种用于多层陶瓷电容器的制备方法，包括：
混合包含主要组分和次要组分的原料粉末以制备介电组合物；
模制和层叠所述介电组合物以制备多层陶瓷片；以及
增塑所述多层陶瓷片，然后在还原气氛下烧制和再氧化所述多层陶瓷片。
6.根据权利要求5所述的用于多层陶瓷电容器的制备方法，其中，所述还原气氛为0.01％至1.0％的H2。
7.根据权利要求5所述的用于多层陶瓷电容器的制备方法，其中，在1150至1250℃的温度下进行所述多层陶瓷片的烧制。
CN2011103501662A 2010-11-08 2011-11-08 具有高介电常数的介电组合物、包括其的多层陶瓷电容器、和多层陶瓷电容器的制备方法 Pending CN102531591A (zh)

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