CN101081734B - 介质陶瓷及叠层陶瓷电容器 - Google Patents

介质陶瓷及叠层陶瓷电容器 Download PDF

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CN101081734B
CN101081734B CN2007100979623A CN200710097962A CN101081734B CN 101081734 B CN101081734 B CN 101081734B CN 2007100979623 A CN2007100979623 A CN 2007100979623A CN 200710097962 A CN200710097962 A CN 200710097962A CN 101081734 B CN101081734 B CN 101081734B
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oxide compound
ceramic
barium titanate
sosoloid
respect
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CN101081734A (zh
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金田和巳
上田周作
池见慎一郎
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Taiyo Yuden Co Ltd
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Abstract

本发明提供一种介质陶瓷及Ni内部电极叠层陶瓷电容器，所述介质陶瓷的可靠性比先前高，且介电常数的温度特性满足X6S特性。本发明的特征在于，以ABO3+aRe+bM+Zr氧化物(其中，ABO3以表示钙钛矿型结构的通式表示钛酸钡系固溶体，Re是从La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及Y中选择的至少1种金属的氧化物，M是从Mg、Al、Cr、Mn、Fe、Ni、Cu及Zn中选择的金属元素的氧化物，a、b表示将各氧化物换算为包含1个金属元素的化学式时的相对于1 mol的ABO3的mol数)表示时，处于1.100≤Ba/Ti≤1.700、0.05≤a≤0.25、0.05≤b≤0.25的范围，Zr氧化物以相对于Ti的Zr的比率表示时，处于Ti∶Zr＝95∶5～60∶40的范围。

Description

介质陶瓷及叠层陶瓷电容器
技术领域
本发明涉及一种以钛酸钡(BaTiO3)为主体的介质陶瓷、以及使用了所述介质陶瓷的叠层陶瓷电容器，且可以获得具有由Ni或Ni合金而构成的内部电极的叠层陶瓷电容器。
背景技术
用于移动装置、通讯装置等电子装置的叠层陶瓷电容器对小型化及大容量化的要求不断提高。为了制造所述小型大容量的叠层陶瓷电容器，提出了例如专利第3567759号公报中所记载的介质陶瓷组成物，所述介质陶瓷组成物包含钛酸钡系固溶体以及添加成分，且于高频·高电压下的损耗及发热较小。
而且，专利第3361531号公报中提出了如下介质陶瓷组成物，即，以钛酸钡为主体，可以在还原环境下与Ni同时烧制，且介电常数较高。
【专利文献1】专利第3567759号公报
【专利文献2】专利第3361531号公报
发明内容
近年来，对叠层陶瓷电容器要求进一步的小型化及大容量化，烧制后的陶瓷层的厚度进一步达到10μm以下，进而达到5μm以下的级别。专利第3567759号公报中所示的介质陶瓷组成物中，在所述公报的实施例中记载的生片厚度20μm的级别下，高温负荷寿命较长，具有充分的可靠性，但存在如下问题：烧制后的陶瓷层的厚度进一步达到10μm以下的级别时，可靠性降低。
而且，近年来要求失真较小的低失真电容器，但专利第3361531号公报中所示的介质陶瓷组成物中，介电常数较高，为7000以上，虽然适于大容量化，但是不适于低失真电容器的用途。
本发明的目的在于提供一种介质陶瓷及Ni内部电极叠层陶瓷电容器，所述介质陶瓷的可靠性比先前高，介电常数的温度特性满足X6S特性，且介电常数为250～850。
本发明提出一种介质陶瓷，其特征在于其是包含主成分、以及SiO2或以SiO2为主体的玻璃成分的烧结体，且所述SiO2或以SiO2为主体的玻璃成分相对于所述钛酸钡系固溶体100重量份，处于1.0～10.0重量份的范围内，其中所述主成分以ABO3+aRe+bM+Zr氧化物(其中，ABO3以表示钙钛矿型结构的通式表示钛酸钡系固溶体，Re是从La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及Y中选择的至少1种金属的氧化物，M是从Mg、Al、Cr、Mn、Fe、Ni、Cu及Zn中选择的金属元素的氧化物，a、b表示将各氧化物换算为包含1个金属元素的化学式时的相对于1mol的ABO3的mol数)表示时，处于1.100≤Ba/Ti≤1.700、0.05≤a≤0.25、0.05≤b≤0.25的范围，Zr氧化物以相对于Ti的Zr的比率表示时，处于Ti∶Zr＝95∶5～60∶40的范围。进而，以Sr或Ca取代所述钛酸钡系固溶体的Ba的一部分。
此外，Ba/Ti比表示钛酸钡系固溶体中所含有的Ba与Ti的比，并非必须与钙钛矿型结构中的A/B比一致。例如以BaTiO3与(Ba1-x-yCaxSry)TiO3为例，任一个的A/B比均为1，但关于Ba/Ti比，BaTiO3为1，而(Ba1-x-yCaxSry)TiO3为1-x-y。
而且，本发明提出一种叠层陶瓷电容器，其具有多个介质陶瓷层、形成在该介质陶瓷层间的内部电极、以及与该内部电极电连接的外部电极，其特征在于所述介质陶瓷层由如上所述的介质陶瓷而构成，且所述内部电极由Ni或Ni合金而形成。
根据本发明，可以获得如下介质陶瓷，其可以在1280℃以下烧制，介电常数为250～850，且构成温度特性满足X6S的Ni内部电极叠层陶瓷电容器。
而且，本发明可以通过特别指定Ba/Ti，而与先前的介质陶瓷相比使寿命特性等可靠性提高。
而且，本发明的介电常数为250～850左右，可以应用在低失真型叠层陶瓷电容器中。
附图说明
图1是表示叠层陶瓷电容器的剖面的模式图。
[符号的说明]
1叠层陶瓷电容器
2陶瓷叠层体
3介质陶瓷层
4内部电极
5外部电极
6第一镀层
7第二镀层
具体实施方式
以下说明本发明的介质陶瓷的实施形态。本发明的介质陶瓷以所述组成比含有钛酸钡系固溶体、Re(Re是从La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及Y中选择的至少1种金属的氧化物)、M(M是从Mg、Al、Cr、Mn、Fe、Ni、Cu及Zn中选择的金属元素的氧化物)、以及Zr氧化物，且所述介质陶瓷是烧结体，该烧结体将以SiO2或SiO2为主体的玻璃成分作为烧结助剂而添加。作为玻璃成分，列举了Li2O-SiO2系玻璃或B2O3-SiO2系玻璃等。
所述介质陶瓷以如下所述方式而获得。首先，以符合本发明的范围的组成比的方式称量并准备BaCO3、TiO2、ZrO2作为起始物料。此时，亦可以适当准备CaCO3、SrCO3。而且，亦可以使用BaZrO3、CaZrO3、SrZrO3代替ZrO2。向所述各原料中加入水后使用球磨机、玻珠研磨机、分散研磨机等进行湿式混合。使混合后的物质干燥，将干燥后的物质在1100～1250℃下进行预烧，从而获得钛酸钡系固溶体。
将以符合本发明的范围的组成比的方式对Re成分(例如Ho2O3)、M成分(例如MgO及MnO，也可以是MnCO3、Mn3O4)、以及烧结助剂(例如SiO2)进行称量后的物质，加入已获得的钛酸钡系固溶体中，利用球磨机等进行湿式混合、干燥后在700～900℃下进行预烧，从而获得介质陶瓷粉末。所获得的介质陶瓷粉末用于形成叠层陶瓷电容器的介质陶瓷层。
其次说明本发明的实施形态的叠层陶瓷电容器。本实施形态的叠层陶瓷电容器1如图1所示，具有多个介质陶瓷层3；以及陶瓷叠层体2，其包含形成在该介质陶瓷层间的内部电极4。在陶瓷叠层体2的两端面上，以与内部电极电连接的方式形成着外部电极5，且如有必要，在外部电极5上形成第一镀层6、第二镀层7。
其次，说明该叠层陶瓷电容器1的制造方法。首先，准备形成本发明的介质陶瓷的原料粉末。将该原料粉末与丁缩醛系或丙烯酸系有机粘合剂、溶媒、以及其他添加剂混合后，形成陶瓷料浆。使用辊涂机等涂布装置，使该陶瓷料浆形成为薄层，形成作为介质陶瓷层3的具有特定厚度的陶瓷生片。在该陶瓷生片上，通过丝网印刷将Ni或Ni合金的导电膏涂布成特定图案形状，形成作为内部电极4的导体层。
叠层必要张数的形成导体层后的陶瓷生片后，进行压接，形成原始的叠层体。将该叠层体切断分割为各单个小片后，在空气中或氮气等非氧化性气体中，除去粘合剂。除去粘合剂后，在各单个小片的内部电极露出面上涂布导电膏后，形成作为外部电极5的导体膜。在特定温度的氮气—氢气环境中(氧分压为10-10atm左右)，烧制形成该导体膜后的各单个小片。此外，外部电极5可以在烧制各单个小片而形成陶瓷叠层体2后，在内部电极露出面上涂布含有玻璃粉的导电膏后进行烧接。外部电极5除可以使用与内部电极相同的金属外，也可以使用Ag、Pd、AgPd、Cu、Cu合金等。进而，利用Ni、Cu等，在外部电极5上形成第一镀层6，且利用Sn或Sn合金等在第一镀层6上形成第二镀层7，从而获得叠层陶瓷电容器1。
[实施例]
(实施例1)
准备BaCO3、TiO2、ZrO2、Gd2O3、MgO作为起始物料，来获得表1的组成的烧结体。此外，表1中，利用将Ti+Zr设为100时的比来表示Ba、Ti、Zr。
[表1]
Figure S07197962320070508D000041
*本发明范围外
利用球磨机，对已准备的BaCO3、TiO2、ZrO2进行湿式混合，干燥后在1100℃下预烧后获得钛酸钡系固溶体。其次，以成为表1的组成的方式向该钛酸钡系固溶体中添加Gd2O3、MgO、MnO、以及SiO2，利用球磨机进行湿式混合，干燥后在900℃下预烧后获得介质陶瓷粉末。此外，表1中，烧结助剂以相对于钛酸钡系固溶体100重量份的重量份来表示。
向所述粉末中添加并混合聚乙烯醇缩丁醛、有机溶剂、增塑剂，形成陶瓷料浆。利用辊涂机，使该陶瓷料浆形成为薄层，从而获得厚度为5μm的陶瓷生片。利用丝网印刷，在该陶瓷生片上涂布Ni内部电极膏，形成内部电极图案。叠层21张形成内部电极图案后的陶瓷生片，并进行压接，以大小4.0×2.0mm对所述压接后的陶瓷生片进行切断分割，形成原始小片。在氮气环境中，对该原始小片除去粘合剂，涂布Ni外部电极膏，且在还原环境中(氮气—氢气环境、氧分压为10-10atm)，在以表2所示的烧制温度下烧制。对利用如上所述而获得的3.2×1.6mm尺寸、介质陶瓷层的厚度为3μm的叠层陶瓷电容器的εr(介电常数)、tanδ、温度特性、以及作为可靠性评价的平均寿命进行测定，并归纳在表2中。此外，以150℃、25V/μm的负荷，对每15个试样进行平均寿命测量，当绝缘电阻值为1MΩ以下的时间为48小时以上时，所述平均寿命为○。
[表2]
 
试样编号 烧制温度℃ εr tanδ％ TCC 平均寿命
101* 1280 760 0.38 × ×
102 1280 650 0.35 X6S ○
103 1280 430 0.30 X6S ○
104* 1280 - - - -
105* 1280 - - - -
106 1280 510 0.31 X6S ○
107* 1280 400 0.28 X6S ×
根据所述结果，如果Ba/Ti处于1.100～1.700、Ti∶Zr处于95∶5～60∶40的范围内，则可以获得可靠性高、介电常数的温度特性满足X6S特性、且介电常数处于250～850的范围内的介质陶瓷及Ni内部电极叠层陶瓷电容器。此外，试样104、105烧结NG(失败)。
(实施例2)
与实施例1相同，形成介质陶瓷粉末，来获得表3的组成的烧结体。此处，增加Re的添加量来验证该效果。
[表3]
Figure S07197962320070508D000061
*本发明范围外
使所述介质陶瓷粉末与实施例1相同地形成叠层陶瓷电容器，测量εr、tanδ、温度特性、平均寿命，且归纳在表4中。
[表4]
 
试样编号 烧制温度℃ εr tanδ％ TCC 平均寿命
201 1280 300 0.32 X6S ○
202 1280 310 0.30 X6S ○
203 1280 315 0.25 X6S ○
204 1280 330 0.20 X6S ○
205 1280 335 0.22 X6S ○
206 1280 360 0.21 X6S ○
207 1280 380 0.21 X6S ○
208 1280 400 0.22 X6S ○
209 1280 570 0.25 X6R ○
210 1280 600 0.27 X6R ○
211 1280 560 0.30 X6R ○
212 1280 565 0.28 X6R ○
213 1280 560 0.28 X6R ○
214 1280 570 0.30 X6R ○
215 1280 650 0.30 X6R ○
216* 1280 970 0.35 X6S ×
 
217 1280 850 0.32 X6S ○
218 1280 250 0.25 X6S ○
219* 1280 260 0.30 X6S ×
根据所述结果，如果Re的组成比、即a处于0.05≤a≤0.25的范围内，则可以获得可靠性高、介电常数的温度特性满足X6S特性、且介电常数处于250～850的范围内的介质陶瓷及Ni内部电极叠层陶瓷电容器。
(实施例3)
与实施例1相同地形成介质陶瓷粉末，来获得表5的组成的烧结体。此处，增加M的添加量来验证该效果。
[表5]
Figure S07197962320070508D000081
*本发明的范围外
使所述介质陶瓷粉末与实施例1相同地形成叠层陶瓷电容器，测量εr、tanδ、温度特性、平均寿命，且归纳在表6中。
[表6]
 
试样编号 烧制温度℃ εr tanδ％ TCC 平均寿命
301 1280 450 0.35 X6S ○
302 1280 460 0.40 X6S ○
303 1280 380 0.29 X6S ○
304 1280 370 0.31 X6S ○
305 1280 430 0.33 X6S ○
306 1280 420 0.32 X6S ○
307* 1280 530 0.25 × -
308 1280 450 0.20 X6S ○
309 1280 290 0.22 X6S ○
310* 1280 260 0.24 X6S ×
根据所述结果，如果M的组成比、即b处于0.05≤b≤0.25的范围内，则可以获得可靠性高、介电常数的温度特性满足X6S特性、且介电常数处于250～850的范围内的介质陶瓷及Ni内部电极叠层陶瓷电容器。
(实施例4)
与实施例1相同地形成介质陶瓷粉末，来获得表7的组成的烧结体。此处，试样408是专利文献1地实施例，409是众所周知的组成。此外，此处，使用B2O3-SiO2-BaO玻璃作为用作烧结助剂的玻璃成分。
[表7]
Figure S07197962320070508D000091
*本发明的范围外
使所述介质陶瓷粉末与实施例1相同地形成叠层陶瓷电容器，测量εr、tanδ、温度特性、平均寿命，且归纳在表8中。
[表8]
 
试样编号 烧制温度℃ εr tanδ％ TCC 平均寿命
401* 1280 - - - -
402 1280 550 0.25 X6S ○
403 1260 270 0.35 X6S ○
404* 1260 240 0.40 X6S ×
405 1260 330 0.45 X6S ○
406 1280 340 0.25 X6S ○
407 1280 320 0.24 X6S ○
408* 1280 400 0.20 X6S ×
409 1280 6000 0.65 × ○
根据所述结果，如果烧结助剂的组成相对于钛酸钡系固溶体100重量份处于1.0～10.0重量份的范围内，则可以获得可靠性高、介电常数的温度特性满足X6S特性、且介电常数处于250～850的范围内的介质陶瓷及Ni内部电极叠层陶瓷电容器。而且，可知本发明的介质陶瓷及叠层陶瓷电容器具有比先前更优异的特性。
根据以上结果，根据本发明，可以提供比先前的可靠性高、介电常数的温度特性满足X6S特性、且介电常数为250～850的介质陶瓷及Ni内部电极叠层陶瓷电容。

Claims (3)

1.一种介质陶瓷，其特征在于：
其是包含以ABO3+aRe+bM+Zr氧化物表示的主成分、以及SiO2或以SiO2为主体的玻璃成分的烧结体，且介电常数为250～850，
ABO3以表示钙钛矿型结构的通式表示钛酸钡系固溶体，Re是从La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及Y中选择的至少1种金属的氧化物，M是从Mg、Al、Cr、Mn、Fe、Ni、Cu及Zn中选择的金属元素的氧化物，a、b表示将各氧化物换算为包含1个金属元素的化学式时的相对于1mol之ABO3之mol数，
其中
1.100≤Ba/Ti≤1.700
0.05≤a≤0.25
0.05≤b≤0.25
Zr氧化物以相对于Ti的Zr的比率表示时，处于
Ti∶Zr＝95∶5～60∶40
的范围，且所述SiO2或以SiO2为主体的玻璃成分相对于所述钛酸钡系固溶体100重量份，处于1.0～10.0重量份的范围内。
2.根据权利要求1所述的介质陶瓷，其特征在于：
以Sr或Ca取代所述钛酸钡系固溶体的Ba的一部分。
3.一种叠层陶瓷电容器，其具有多个介质陶瓷层、形成在上述介质陶瓷层间的内部电极、以及与所述内部电极电连接的外部电极，所述叠层陶瓷电容器的特征在于：
所述介质陶瓷层是包含以ABO3+aRe+bM+Zr氧化物表示的主成分、以及SiO2或以SiO2为主体的玻璃成分的烧结体，且介电常数为250-850，
ABO3以表示钙钛矿型结构的通式表示钛酸钡系固溶体，Re是从La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及Y中选择的至少1种金属的氧化物，M是从Mg、Al、Cr、Mn、Fe、Ni、Cu及Zn中选择的金属元素的氧化物，a、b表示将各氧化物换算为包含1个金属元素的化学式时的相对于1mol之ABO3之mol数，
其中 
1.100≤Ba/Ti≤1.700
0.05≤a≤0.25
0.05≤b≤0.25
Zr氧化物以相对于Ti的Zr的比率表示时，处于
Ti∶Zr＝95∶5～60∶40
的范围，且所述SiO2或以SiO2为主体的玻璃成分相对于所述钛酸钡系固溶体100重量份，处于1.0～10.0重量份的范围内，
且所述内部电极由Ni或Ni合金而形成。 
CN2007100979623A 2006-04-28 2007-04-25 介质陶瓷及叠层陶瓷电容器 Expired - Fee Related CN101081734B (zh)

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