CN101489952A - 电介质陶瓷、及陶瓷电子部件、以及叠层陶瓷电容器 - Google Patents
电介质陶瓷、及陶瓷电子部件、以及叠层陶瓷电容器 Download PDFInfo
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- CN101489952A CN101489952A CNA2007800258628A CN200780025862A CN101489952A CN 101489952 A CN101489952 A CN 101489952A CN A2007800258628 A CNA2007800258628 A CN A2007800258628A CN 200780025862 A CN200780025862 A CN 200780025862A CN 101489952 A CN101489952 A CN 101489952A
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Abstract
本发明的电介质陶瓷,主成分由用通式{(Ba1-x-yCaxSny)m(Ti1-zZrz)O3}表示的钙钛矿型化合物组成,上述x、y、z及m分别满足0.02≤x≤0.20、0.02≤y≤0.20、0≤z≤0.05、0.99≤m≤1.1,并且在1.0×10-10~1.0×10-12MPa的低氧分压下进行热处理而形成电介质陶瓷。由此,实现一种电介质陶瓷、及使用该电介质陶瓷的叠层陶瓷电容器等陶瓷电子部件,其中,该电介质陶瓷不损害电介质特性,在高温气氛中也能稳定地进行使用,并且容易调整特性,即使共同焙烧陶瓷层和导电膜也不会发生电极断裂。
Description
技术领域
本发明涉及一种电介质陶瓷、及陶瓷电子部件、以及叠层陶瓷电容器,更详细地,涉及一种适于在高温气氛中使用的电介质陶瓷、及使用该电介质陶瓷的陶瓷电子部件以及叠层陶瓷电容器。
背景技术
近年来,叠层陶瓷电容器等各种陶瓷电子部件被广泛地搭载在汽车用的电子控制设备等各种电子设备中。
作为在这种陶瓷电子部件中使用的电子材料,到目前为止,众所周知一种主成分为钛酸钡(BaTiO3)的电介质陶瓷材料,并正积极进行研究·开发。
例如,在专利文献1中,提出了一种电介质陶瓷合成物,作为其必备主成分在规定组成范围内含有BaO、TiO2、SnO2、Bi2O3、MgO及SiO2;作为其选择的必备成分在规定的范围内含有La2O3、Sm2O3、及Nd2O3内的至少1种。
在此专利文献1中,由于使上述必备主成分及选择的必备成分为规定范围,所以得到相对介电常数ε r为1000以上、介质损耗tan δ为10%以下的适于所谓延迟线用途的使用的电介质陶瓷合成物。
此外,在专利文献2中提出了一种电介质陶瓷合成物,其以由组成式:(Ba1-xSnx)mTiO3表示的钙钛矿型化合物为主成分,x及m处于0.01≤x≤0.3、0.9≤m≤1.1的范围内,并且由上述(Ba1-xSnx)表示的Ba位实质上不含Sr。
在此专利文献2中,在规定摩尔范围内将BaTiO3的Ba的一部分替换为Sn,并且通过混合以便使得Ba位和Ti位的摩尔比成为规定范围,来得到具有130℃以上的居里温度(Curie temperature)Tc、约20μC/cm2以上的剩余极化、及700以上的较高的相对介电常数ε r的非铅类的电介质陶瓷合成物。
再有,由于Sn通常作为4价的阳离子维持稳定的状态,所以认为在BaTiO3类化合物中,Sn通常固溶于Ti位中。此外,在非专利文献1中记载了,虽然BaTiO3的居里温度Tc是120℃,但在用Sn替换Ti的一部分的情况下,居里温度Tc从120℃大幅降低到室温以下。
专利文献1:JP特开平3—040962号公报
专利文献2:国际公开第2005/075377号小册子
非专利文献1:岡崎清著、「セラミツク誘電体工学」、第3版、学献社、1983年6月、p.281—283
发明内容
专利文献1的电介质陶瓷合成物,由于居里温度Tc低为—20~+15℃,由于温度上升导致相对介电常数ε r急剧减少,所以在实用中存在所谓在高温气氛下使用困难的问题。特别地,由于叠层陶瓷电容器最近广泛用于汽车用途,所以要求即使在150℃左右的高温气氛下也能稳定使用。
再有,认为专利文献1的电介质陶瓷合成物如上所述居里温度Tc低为—20~+15℃,这是因为如果考虑上述非专利文献1的记载,则Sn固溶于Ti位中。
另一方面,在专利文献2的电介质陶瓷合成物中,通过使Sn固溶于Ba位,则得到130℃以上的较高的居里温度Tc。
但是,在专利文献2中,由于焙烧时的氧分压非常低为10-12~10-16MPa,所以焙烧条件的自由度变窄,存在所谓陶瓷电子部件的特性调整困难的问题。此外,由于焙烧温度的变化等导致电介质陶瓷的绝缘性下降。并且,在叠层陶瓷电容器中使用此电介质陶瓷合成物的情况下,当使内部电极薄层化时,则会在共同焙烧成为内部电极的导电膜和陶瓷层时使导电性材料球状化,产生所谓的电极断裂,恐怕存在上述这样的问题。
即,Sn通常以4价维持稳定的状态,但为了使Sn固溶于Ba位,有必要使其为2价。为此,在专利文献2中,在使氧分压为非常低的10-12~10-16MPa的还原气氛中进行焙烧处理。但是,在其另一方面,由于焙烧时的氧分压如上述那样非常低,所以焙烧条件的自由度变窄,因焙烧温度的变化等导致电介质陶瓷的绝缘性下降,进而导致内部电极的电极断裂,恐怕存在上述这样的问题。
鉴于这样的情况进行本发明,其目的在于,提供一种不有损电介质特性、即使在高温气氛中也能稳定的使用并且容易进行特性调整、即使共同焙烧陶瓷层和导电膜也不产生电极断裂的电介质陶瓷、及使用此电介质陶瓷的陶瓷电子部件,以及叠层陶瓷电容器。
在BaTiO3类化合物中,通过使Sn固溶于Ba位,就能够使居里温度Tc上升。但是,为了将以4价稳定的Sn还原为2价并使其固溶于Ba位,而如专利文献2那样,使焙烧时的氧分压非常低为10-12~10-16MPa时,就产生上述这样各种问题。
然而,本发明者们的锐意研究的结果,可知如果合成物中含有Ca,则此Ca就会促进Sn向Ba位固溶。而且,其结果,得到以下的知识,即使不在10-12~10-16MPa的极端低的氧分压下进行焙烧处理,也能够得到居里温度Tc较高的电介质陶瓷。此外,为了平稳地进行Sn从4价向2价的还原,考虑希望在规定范围的低氧分压下进行不仅包含焙烧时而且还包含煅烧时的热处理工序。
根据这样的知识进行本发明,本发明相关的电介质陶瓷,其特征在于,主成分由用通式{(Ba1-x-yCaxSny)m(Ti1-zZrz)O3}表示的钙钛矿型化合物组成,上述x、y、z及m分别满足0.02≤x≤0.20、0.02≤y≤0.20、0≤z≤0.05、0.99≤m≤1.1。
此外,本发明的电介质陶瓷,其特征在于,居里温度是130℃以上。
并且,本发明的电介质陶瓷,其特征在于,与100摩尔份上述主成分相比,含有0.02~2摩尔份Mn及V的至少任意一种成分。
此外,本发明的电介质陶瓷,其特征在于,与100摩尔份上述主成分相比,含有0.02~5摩尔份Si。
此外,本发明相关的陶瓷电子部件,其特征在于,由上述电介质陶瓷形成的陶瓷基体包括导体。
并且,本发明相关的叠层陶瓷电容器,具有交替层叠陶瓷层和内部电极的烧结而成的陶瓷基体,并且在该陶瓷基体的两端部形成外部电极,电连接该外部电极和上述内部电极;上述叠层陶瓷电容器中,其特征在于,其中上述陶瓷层由上述电介质陶瓷形成。
发明效果
根据本发明的电介质陶瓷,由于Ca促进Sn向Ba位固溶,所以即使不在极端低的氧分压下进行热处理,也能够得到具有高居里温度Tc的电介质陶瓷。并且,由此,能够得到即使在高温气氛中也具有稳定的电介质特性,并且扩大焙烧条件的自由度而容易进行特性调整,可回避导致绝缘性下降等的电介质陶瓷。
此外,由于居里温度是130℃以上,所以能够得到适于要求在约150℃的高温气氛中的稳定使用的汽车等的用途的电介质陶瓷。
此外,由于与100摩尔份上述主成分相比,含有0.02~2摩尔份Mn及V的至少任意一种成分,或者与100摩尔份上述主成分相比,含有0.02~5摩尔份Si,所以能够提高烧结性。
此外,根据本发明的陶瓷电子部件,由于由上述电介质陶瓷形成的陶瓷基体包括导体,所以能够实现如下陶瓷电子部件,其可在高温气氛中稳定的使用,而且通过焙烧条件的调整能够容易地改变电介质特性,不会因焙烧温度变动等而导致绝缘性下降。
此外,根据本发明的叠层陶瓷电容器,由于陶瓷层由上述电介质陶瓷形成,所以能够使焙烧气氛的氧分压为约10-10~10-12MPa进行焙烧,因此除上述作用效果外,即使减薄内部电极的厚度,也能够抑制因内部电极的球状化而产生的电极断裂等不合格。因此,能够容易地实现可在高温气氛中稳定使用、适于汽车用途等的叠层陶瓷电容器。
附图说明
图1是示意地表示作为使用本发明相关的电介质陶瓷的陶瓷电子部件的叠层陶瓷电容器的一个实施方式的剖面图。
符号说明
1 陶瓷基体 2a~2d 内部电极
3a、3b 外部电极 6a~6e 陶瓷层(电介质陶瓷)
具体实施方式
接着,详细说明本发明的实施方式。
本发明的一实施方式相关的电介质陶瓷,主成分由用下述通式(A)表示的钙钛矿型化合物组成。
(Ba1-x-yCaxSny)m(Ti1-zZrz)O3 …(A)
在此,x、y、z及m满足下述式子(1)~(4)。
0.02≤x≤0.20 …(1)
0.02≤y≤0.20 …(2)
0≤z≤0.05 …(3)
0.99≤m≤1.1 …(4)
即,本电介质陶瓷,主成分由具有钙钛矿型构造的BaTiO3类化合物形成,同时在规定摩尔范围内将Ba位的Ba的一部分替换为Sn及Ca。
如此,通过使Sn作为2价阳离子固溶于Ba位,就能够使居里温度Tc成为130℃以上的高温,能够得到即使在约150℃的高温气氛中也可稳定使用的电介质陶瓷。
并且,由于用Ca替换Ba的一部分,所以即使未将焙烧气氛设定为极低的氧分压(例如,1.0×10-12~1.0×10-16MPa)也能够得到所希望的电介质陶瓷。
以下详述将上述x、y、z及m限定在式子(1)~(4)的范围内的理由。
(1)x
如上所述,通过使BaTiO3类化合物中含有Ca,就能够促进Sn向Ba位固溶。例如,通过在约1.0×10-10~1.0×10-12MPa的低氧分压下的焙烧,就能够使Sn固溶于Ba位中。
但是,Ba位中的Ca的摩尔比x不到0.02的情况下,Ca的摩尔含量过少,不能充分促进Sn向Ba位固溶。另一方面,当上述摩尔比x超过0.20时,会导致烧结性下降,不优选。
因此,在本实施方式中,按使摩尔比x为0.02≤y≤0.20来配合组成成分。
(2)y
虽然BaTiO3的居里温度Tc是120℃(非专利文献1),但通过使Sn固溶于Ba位,也能够使居里温度Tc上升到130℃以上。
但是,Ba位中的Sn的摩尔比y不到0.02的情况下,由于Sn的摩尔含量过少,所以不能期待居里温度Tc的上升效果。另一方面,当上述摩尔比y超过0.20时,虽然居里温度Tc会上升,但相对介电常数ε r为下降趋势,介质损耗tan δ也变大。
因此,在本实施方式中,按使摩尔比y为0.02≤y≤0.20来配合组成成分。
(3)z
在本电介质陶瓷中可以根据需要用Zr替换Ti的一部分。
但是,当Ti位中的Zr的摩尔比z超过0.05时,居里温度Tc就会显著下降,不能得到可在高温气氛中稳定使用的电介质陶瓷。
因此,在本实施方式中,按使摩尔比z为0≤y≤0.05来配合组成成分。
(4)m
虽然Ba位和Ti位的摩尔比m在化学计量成分(stoichiometriccomposition)中是1.00,但也优选根据需要从化学计量成分进行变位。
但是,当上述摩尔比m从化学计量成分进行变位而不到0.99时或超过1.1时,恐怕会导致烧结性下降。
因此,在本实施方式中,按使摩尔比m为0.99≤m≤1.1来配合组成成分。
再有,作为Ca在电介质陶瓷中的存在形式,虽然如上所述Ca固溶于Ba位,但由于Ca几乎不影响居里温度Tc的增减,所以在不影响其它各特性的范围内既可以存在于晶体边界(crystalline boundary)和晶体三相点(crystalline triple point),也可以固溶于Ti位。
再有,基于使烧结性提高的观点,优选在主成分中添加Mn及V的至少任意一种成分。此情况下,为了得到提高烧结性的效果,优选与100摩尔份主成分相比,含有至少0.02摩尔份以上。但是,当与100摩尔份主成分相比超过2摩尔份时,电介质特性会有下降趋势。因此,添加Mn和V时的含量优选与100摩尔份主成分相比为0.02~2摩尔份。
此外,基于同样的理由,优选与100摩尔份主成分相比,含有0.02~5摩尔份的Si。
再有,在本发明中,优选居里点(Curie point)是130℃以上。在本发明的电介质陶瓷中,由于其主成分中含Sn,所以通过确认居里温度是130℃,就可旁证Sn位于Ba位。也如上述非专利文献1所示的,是因为Sn位于Ti位的时候,居里温度会从120℃大大下降。
此外,虽然由于本发明的电介质陶瓷用Sn替换Ba位的一部分,有利于得到较高的居里温度,但不希望大量含有使居里温度下降这样的成分。即便在添加使居里温度下降的成分的情况下,也希望通过增多向Ba位的Sn的替换量等手段进行补偿。
相反,作为Sn以外使钛酸钡的居里温度上升的元素,可列举Pb和Bi。但是,由于Pb和Bi是环境负担物质,并且耐还原性非常弱,所以在叠层陶瓷电容器中很难采用。基于以上内容,在本发明的电介质陶瓷中,通过确认居里温度是135℃以上,实质上就能证明Sn作为2价阳离子位于Ba位。
图1是表示使用上述电介质陶瓷的叠层陶瓷电容器的一实施方式的剖面图。
在陶瓷基体1中埋设内部电极2a~2d,同时在该陶瓷基体1的两端面上形成外部电极3a、3b,并且用第1电镀被膜4a、4b及第2电镀被膜5a、5b覆盖上述外部电极3a、3b,如此这样形成该叠层陶瓷电容器。
即,交替层叠用本发明的电介质陶瓷形成的陶瓷层6a~6e和内部电极2a~2d,经焙烧成为陶瓷基体1,内部电极层2a、2c与外部电极3a电连接,内部电极层2b、2d与外部电极3b电连接。并且,在内部电极层2a、2c和内部电极层2b、2d的对置面间形成静电容量。
接着,详述上述叠层陶瓷电容器的制造方法。
首先,作为陶瓷原材料,准备BaCO3等的Ba化合物、TiO2等的Ti化合物、CaCO3等的Ca化合物、SnO2等的Sn化合物,根据需要准备ZrO2等Zr化合物。
接着,称量上述陶瓷原材料,以使上述通式(A)满足上述式子(1)~(4)。
接着,将此称量物与PSZ(Partially Stabilized Zirconia:部分稳定氧化锆)球等卵石及纯水一起投入球磨机中,湿式地充分地混合粉碎后,以约1000℃以上的温度实施煅烧处理(热处理),制作主成分粉末。在此,由于作为煅烧气氛,需要将4价的Sn还原为2价,所以希望是由氧分压为1.0×10-10~1.0×10-12MPa的N2-H2混合气体构成的还原气氛。
接着,准备作为副成分材料的MnO等Mn化合物、V2O5等V化合物,SiO2等Si化合物,在球磨机内混合这些副成分材料和上述主成分粉末,此后使其蒸发干燥,得到陶瓷原料粉末。再有,由于副成分材料的添加是任意的,所以不添加副成分材料的时候可以省略此工序。
接着,将上述陶瓷原料粉末与有机粘合剂和有机溶剂一起投入球磨机中进行湿式混合,由此制作陶瓷浆料,此后,利用刮刀法等对陶瓷浆料实施成型加工,制作陶瓷生片。
接着,使用内部电极用导电膏在陶瓷生片上施行丝网印刷,在上述陶瓷生片的表面上形成规定图形的导电膜。
再有,作为内部电极用导电膏中所含的导电性材料,基于低成本化的观点,优选使用Ni、Cu、Ag和它们的合金。
接着,按规定方向层叠多片形成了导电膜的陶瓷生片,用未形成导电膜的陶瓷生片夹持、压接、以规定尺寸切断,制作陶瓷叠层体。而且此后,以温度约300~500℃的温度进行脱粘合剂处理,并且在由将氧分压控制在约1.0×10-10~1.0×10-12MPa的H2-N2-H2O混合气体构成的还原性气氛下,以温度1000~1200℃进行约2小时焙烧处理(热处理)。由此,共同焙烧导电膜和陶瓷生片,得到交替层叠了内部电极2a~2d和陶瓷层6a~6e的陶瓷基体1。
接着,在陶瓷基体1的两端面上涂敷外部电极用导电膏,进行烘焙处理,由此,形成外部电极3a、3b。
再有,外部电极用导电膏优选使用在导电性材料中添加了玻璃粉的物质。此外,作为导电性材料,基于低成本化的观点,能够使用Ni、Cu、Ag和它们的合金,并且按照要求能够使用Pd、Ag-Pd等。
此外,作为外部电极3a、3b的形成方法,也可以在陶瓷叠层体的两端面上涂敷外部电极用导电膏后,与陶瓷叠层体同时实施焙烧处理。
接着,对外部电极3a、3b的表面实施电解电镀,形成由Ni、Cu、Ni-Cu合金等构成的第1电镀被膜4a、4b,并且为了得到良好的焊接性,对上述第1电镀被膜4a、4b的表面实施电解电镀,形成由焊料和锡等构成的第2电镀被膜5a、5b,由此制造叠层陶瓷电容器。
再有,本发明不限于上述实施方式。在上述实施方式中,虽然在煅烧合成时得到所希望的主成分粉末,但也可以调合Ba位和Ti位的摩尔比m使其比预定量更少,并进行煅烧处理,此后,可以适当添加不足成分制作所希望的主成分粉末。此情况下,作为不足成分所添加的成分,由于主要通过焙烧固溶于Ba位,所以能够满足所希望的m值。
此外,在上述实施方式中,作为陶瓷电子部件的一例,虽然例示出叠层陶瓷电容器,但毫无疑问,对于单片陶瓷电容器和其它的陶瓷电子部件也同样能够适用。
接着,具体地说明本发明的实施例。
实施例1
首先,作为陶瓷原材料准备BaCO3、TiO2、CaCO3及SnO2。然后,称量这些陶瓷原材料以使主成分为表1这样的组成。接着,将这些称量物与PSZ球和纯水一起投入球磨机中,湿式地充分混合粉碎,经干燥得到混合粉体。
接着,在将氧分压调整到约1.0×10-10.0MPa的N2-H2混合气体的还原气氛下,以1000℃的温度实施2小时热处理,煅烧此混和粉末,此后,干式粉碎,制作主成分组成由(Ba1-x-yCaxSny)mTiO3表示的陶瓷原料粉末。
接着,以乙醇为溶剂,加入聚乙烯醇缩丁醛(ポロビニルブチラ—ル:poly(vinyl butyral))类粘合剂混合粉碎此陶瓷原料粉末,得到陶瓷浆料。然后,使用刮刀法对上述陶瓷浆料施行成型加工,得到陶瓷生片。
接着,在陶瓷生片的表面上丝网印刷主成分为Ni的导电膏,形成导电膜。接着,按规定的方向层叠形成了此导电膜的陶瓷生片,用未形成导电膜的陶瓷生片夹持、压接、制作出陶瓷叠层体。
接着,在氮气氛中,以温度350℃的温度加热此陶瓷叠层体,燃烧去除粘合剂,此后,在由调整到表1所示的氧分压的H2-N2-H2O气体构成的还原性气氛下,以1200℃的温度实施2小时焙烧处理(热处理)得到陶瓷基体(陶瓷烧结体)。
接着,在此陶瓷基体的两端面上涂敷以含B-Li-Si-Ba-O类玻璃粉的Cu为主成分的导电膏,在氮气氛中以600℃的温度进行烘焙处理,形成与内部电极电连接的外部电极。
而且,最后实施电解电镀在外部电极的表面上形成Ni被膜及Sn被膜,由此制作出样品编号1~6的叠层陶瓷电容器。
再有,这些叠层陶瓷电容器的外形尺寸为长2.0mm、宽1.0mm、厚0.5mm。此外,插入内部电极间的陶瓷层的厚度为5μm,内部电极层的厚度是0.5μm,获取静电容量的有效陶瓷层数是5,陶瓷层每一层的对置电极面积为1.3mm2。
接着,测量这些样品编号1~6的各样品的相对介电常数ε r、介质损耗tan δ以及居里温度Tc。
即,使用自动桥式测量仪器,以频率1kHz、有效电压0.2Vrms、温度25℃的条件,测量静电容量C及介质损耗tan δ,基于静电容量C计算出相对介电常数ε r。
此外,在—55~+200℃的范围下测量静电容量的温度变化,以静电容量最大时的温度为居里温度。
此外,用扫描型电子显微镜观察样品编号1~6的样品的剖面,调查内部电极是否球状化。
表1示出了样品编号1~6的组成成分和其测量结果。
[表1]
*本发明范围外
样品编号1,摩尔比x是0.00、居里温度Tc降低到90℃。可认为这是因为虽然调合Sn使摩尔比y为0.05,但由于不含Ca,所以焙烧时的氧分压为1.0×10-10.0MPa下,大部分固溶于Ti位。
样品编号2,虽然居里温度高为145℃,但构成内部电极的Ni(导电性材料)球状化。即,虽然在电介质陶瓷中不含Ca,但由于使焙烧时的氧分压非常低为1.0×10-13.0MPa,所以Sn固溶于Ba位,其结果居里温度Tc上升。但是,另一方面,由于氧分压如上所述非常的低,所以导致Ni球状化。
相对于此,样品编号3~6,摩尔比x为0.02~0.04,由于电介质陶瓷中在本发明范围内含有Ca,所以即使焙烧时的氧分压约为1.0×10-10.0~1.0×10-11.5MPa也不会导致内部电极的球状化,能够得到145℃的较高的居里温度Tc。可认为这是因为合成物中含有Ca,所以促进Sn向Ba位固溶,其结果即使在氧分压:1.0×10-10.0~1.0×10-11.5MPa下焙烧,大部分的Sn也固溶于Ba位。
实施例2
与[实施例1]相同,作为陶瓷原材料准备BaCO3、TiO2、CaCO3及SnO2。然后,称量这些陶瓷原材料以使主成分为表2这样的组成。接着,将这些称量物与PSZ球和纯水一起投入球磨机中,湿式地充分混合粉碎,经干燥得到混合粉体。
接着,在调整到表2所示的煅烧时氧分压的N2-H2混合气体的还原气氛中,以1000℃的温度实施2小时热处理,煅烧此混和粉末,此后,进行干式粉碎,制作出主成分组成由(Ba1-x-yCaxSny)mTiO3表示的陶瓷原料粉末。
接着,以乙醇为溶剂,在此陶瓷原料粉末中加入丙烯酸类有机粘合剂,进行湿式混合,此后干燥、造粒。然后,对此造粒物施加196MPa的压力压制成型,得到直径12mm、厚1mm的圆板状的陶瓷成型体。
接着,在氮气氛中,以350℃的温度加热此陶瓷成型体,燃烧去除粘合剂,此后,在由调整到表2所示的焙烧时氧分压的H2-N2-H2O气体构成的还原性气氛下,以1200℃的温度实施2小时焙烧处理,得到陶瓷基体(陶瓷烧结体)。
接着,使用真空蒸镀法,在上述陶瓷基体的两主表面上形成主成分为Ag的外部电极,制作出样品编号11~19的单片陶瓷电容器。
再有,这些单片陶瓷电容器的外形尺寸为直径10mm、厚0.8mm。
接着,以与[实施例1]相同的方法,测量这些样品编号11~19的各样品的相对介电常数ε r、介质损耗tan δ以及居里温度Tc。
此外,使用X射线衍射装置,对陶瓷基体的表面进行X射线衍射,求室温中的钙钛矿晶体构造的c轴和a轴的轴比c/a。
表2示出了样品编号11~19的组成成分和其测量结果。
[表2]
*本发明范围外
样品编号11,由于在大气气氛中进行煅烧及焙烧,并且不含Sn,所以居里温度Tc与BaTiO3大致相同为120℃。
样品编号12,尽管调整Sn的摩尔比y为0.02,但居里温度Tc也降低为105℃。可认为这是因为由于在大气气氛中进行煅烧及焙烧,所以未还原Sn,以固溶于Ti位为主,其结果居里温度Tc比BaTiO3还低。
样品编号13,虽然调整Sn的摩尔比y为0.02,并且焙烧时的氧分压降低为1.0×10-11.5MPa,但居里温度Tc,也与样品编号12大致相同,为105℃。可认为这是因为虽然在1.0×10-11.5MPa的低氧分压下进行焙烧处理,但由于在大气气氛下进行煅烧处理,所以未充分还原Sn,以固溶于Ti位为主,由此,与样品编号12相同,居里温度Tc比BaTiO3还低。
另一方面可知,样品编号19,虽然煅烧时在1.0×10-10MPa、焙烧时在1.0×10-11.5MPa的低氧分压下分别进行热处理,但由于Sn的摩尔比y是0.30,超过0.20,所以虽然居里温度Tc高为200℃,但相对介电常数εr降低到700,介质损耗tan δ变大为15.0%,导致电介质特性的下降。
相对于此,样品编号14~18,含有Ca摩尔比x为0.13,含有Sn摩尔比y为0.02~0.20,任何一个都处于本发明范围。因此,促进Sn向Ba位固溶,即使在煅烧时:1.0×10-10MPa、焙烧时:1.0×10-11.5MPa的适度的低氧分压下分别进行热处理,也不会导致电介质特性的下降,能够使居里温度Tc上升到130~185℃。
此外,随着居里温度Tc的上升,轴比c/a增加,晶系由立方晶系(cubicsystem)转位为正方晶系(tetragonal system)。因此,在因相对介电常数εr的温度变化而使得最大点不明确的情况下,通过测量轴比c/a,就能够推测居里温度Tc。
实施例3
通过与[实施例1]相同的方法·程序,制作主成分按表3这样的组成调合的样品编号21~29的叠层陶瓷电容器。再有,在本实施例3中,将煅烧时及焙烧时的氧分压任何一个都设定为1.0×10-10MPa,分别进行热处理。
接着,用与[实施例1]相同的方法测量这些样品编号21~29的各样品的相对介电常数ε r、介质损耗tan δ以及居里温度Tc。
表3示出了样品编号21~29的组成成分和其测量结果。
[表3]
*本发明范围外
样品编号25,由于Ba位中的Ca的摩尔比x是0.21,超过了0.20,所以为烧结不良,无法测量特性。
样品编号26,由于Ba位和Ti位的比m是0.98,不到0.99,所以与样品编号25相同,为烧结不良,无法测量特性。
样品编号29,由于Ba位和Ti位的比m是1.15,超过1.1,所以与样品编号25、26相同,为烧结不良,无法测量特性。
相对于此可确认,样品编号21~24、27及28,摩尔比x、y、m任何一个都在本发明范围内,即使在1.0×10-10MPa的氧分压下煅烧·焙烧,也能得到不有损电介质特性、居里温度Tc为150~155℃的叠层陶瓷电容器。
Claims (6)
1.一种电介质陶瓷,
主成分由用通式{(Ba1-x-yCaxSny)m(Ti1-zZrz)O3}表示的钙钛矿型化合物组成,
上述x、y、z及m分别满足
0.02≤x≤0.20、
0.02≤y≤0.20、
0≤z≤0.05、
0.99≤m≤1.1。
2.根据权利要求1所述的电介质陶瓷,其特征在于,居里温度是130℃以上。
3.根据权利要求1或2所述的电介质陶瓷,其特征在于,与100摩尔份上述主成分相比,含有0.02~2摩尔份Mn及V的至少任意一种成分。
4.根据权利要求1至3中任一项所述的电介质陶瓷,其特征在于,与100摩尔份上述主成分相比,含有0.02~5摩尔份Si。
5.一种陶瓷电子部件,其特征在于,由权利要求1至权利要求4中任意一项所述的电介质陶瓷形成的陶瓷基体包括导体。
6.一种叠层陶瓷电容器,具有交替层叠陶瓷层和内部电极的烧结而成的陶瓷基体,并且在该陶瓷基体的两端部形成外部电极,电连接该外部电极和上述内部电极;其特征在于,
上述陶瓷层由权利要求1至权利要求4中任意一项所述的电介质陶瓷形成。
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CN104508772B (zh) * | 2012-08-07 | 2017-09-01 | 株式会社村田制作所 | 层叠陶瓷电容器以及层叠陶瓷电容器的制造方法 |
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US9525123B2 (en) | 2012-11-02 | 2016-12-20 | Canon Kabushiki Kaisha | Piezoelectric material, piezoelectric element, multilayered piezoelectric element. Liquid discharge heard, liquid discharge apparatus, ultrasonic motor, optical apparatus, vibratory apparatus, dust removing device, image pickup apparatus, and electronic equipment |
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JP5131595B2 (ja) | 2013-01-30 |
DE112007001335T5 (de) | 2009-05-20 |
KR101083553B1 (ko) | 2011-11-14 |
US7595975B2 (en) | 2009-09-29 |
JPWO2008004393A1 (ja) | 2009-12-03 |
US20090128989A1 (en) | 2009-05-21 |
WO2008004393A1 (fr) | 2008-01-10 |
DE112007001335B4 (de) | 2019-05-23 |
TW200812931A (en) | 2008-03-16 |
KR20090015146A (ko) | 2009-02-11 |
DE112007001335T9 (de) | 2016-12-22 |
TWI346095B (zh) | 2011-08-01 |
CN101489952B (zh) | 2013-05-01 |
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