CN111312517A - 陶瓷原料粉末、层叠陶瓷电容器及层叠陶瓷电容器的制造方法 - Google Patents
陶瓷原料粉末、层叠陶瓷电容器及层叠陶瓷电容器的制造方法 Download PDFInfo
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- CN111312517A CN111312517A CN201911248733.6A CN201911248733A CN111312517A CN 111312517 A CN111312517 A CN 111312517A CN 201911248733 A CN201911248733 A CN 201911248733A CN 111312517 A CN111312517 A CN 111312517A
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Abstract
本申请提供一种陶瓷原料粉末,其包括:具有钙钛矿结构的主相,其中作为施主的元素和作为受主的元素固溶在钙钛矿结构的B位中,其中在陶瓷原料粉末的各颗粒的中心区域中,满足(作为施主的元素的浓度)×(作为施主的元素的价数‑4)<(作为受主的元素的浓度)×(4‑作为受主的元素的价数)的关系,其中在陶瓷原料粉末的各颗粒的外缘区域中,满足(作为施主的元素的浓度)×(作为施主的元素的价数‑4)>(作为受主的元素的浓度)×(4‑作为受主的元素的价数)的关系。
Description
技术领域
本发明的某个方面涉及陶瓷原料粉末、层叠陶瓷电容器和层叠陶瓷电容器的制造方法。
背景技术
层叠陶瓷电容器具有其中每个电介质层和每个内部电极层交替层叠的结构。电介质层通过烧结陶瓷原料粉末而形成。因此,从层叠陶瓷电容器的良好性能的角度出发,优选陶瓷原料粉末具有预定特性。例如,公开了一种技术,其中预先将预定元素固溶在陶瓷原料粉末中,以便即使减小电介质层的厚度也实现足够的可靠性(例如,参见日本专利申请公开第2017-108128号(在下文中称为文献1)和日本专利申请公开第2017-228737号(在下文中称为文献2))。
发明内容
在文献1中,使用其中固溶有施主元素的钛酸钡。利用该技术,尽管由于施主效应而改善了层叠陶瓷电容器的寿命,但是绝缘特性的降低可能成为问题。在文献2中,使用其中固溶有施主元素和受主元素的钛酸钡。然而,利用该技术,尽管可以抑制绝缘特性的降低,但是施主效应可能降低。
本发明的目的是提供能够实现施主效应和受主效应的陶瓷原料粉末、层叠陶瓷电容器和层叠陶瓷电容器的制造方法。
根据本发明的一方面,提供陶瓷原料粉末,其包含:具有钙钛矿结构的主相,其中作为施主的元素和作为受主的元素固溶在钙钛矿结构的B位中,其中在陶瓷原料粉末的各颗粒的中心区域中,满足(作为施主的元素的浓度)×(作为施主的元素的价数(valence)-4)<(作为受主的元素的浓度)×(4-作为受主的元素的价数)的关系,其中在陶瓷原料粉末的各颗粒的外缘区域中,满足(作为施主的元素的浓度)×(作为施主的元素的价数-4)>(作为受主的元素的浓度)×(4-作为受主的元素的价数)的关系。
根据本发明的另一方面,提供一种层叠陶瓷电容器的制造方法,该方法包括:形成包括陶瓷原料粉末的生片的步骤,该陶瓷原料粉末的主相具有钙钛矿结构;通过交替层叠每个生片和每个用于内部电极的糊料,形成层叠结构的步骤;和烧制层叠结构的步骤,其中作为施主的元素和作为受主的元素固溶在钙钛矿结构的B位中,其中在陶瓷原料粉末的各颗粒的中心区域中,满足(作为施主的元素的浓度)×(作为施主的元素的价数-4)<(作为受主的元素的浓度)×(4-作为受主的元素的价数)的关系,其中在陶瓷原料粉末的各颗粒的外缘区域中,满足(作为施主的元素的浓度)×(作为施主的元素的价数-4)>(作为受主的元素的浓度)×(4-作为受主的元素的价数)的关系。
根据本发明的另一方面,提供一种层叠陶瓷电容器,其包括:多个电介质层;和多个内部电极层,其中多个电介质层中的每一个和多个内部电极层中的每一个交替层叠,其中多个电介质层通过烧制上述陶瓷原料粉末而形成。
附图说明
图1示出层叠陶瓷电容器的透视图,其中示出层叠陶瓷电容器的局部的截面;
图2A和图2B示出作为施主的元素和作为受主的元素的浓度梯度;且
图3示出层叠陶瓷电容器的制造方法。
具体实施方式
将参照附图对实施方式进行说明。
(实施方式)图1示出根据实施方式的层叠陶瓷电容器100的透视图,其中示出层叠陶瓷电容器100的局部的截面。如图1所示,层叠陶瓷电容器100包括具有长方体形状的层叠芯片10以及分别设置在层叠芯片10的彼此面对的两个端面处的一对外部电极20a和20b。在层叠芯片10的四个面中,除了两个端面以外,将层叠芯片10的层叠方向上的上下两面以外的两个面称为侧面。外部电极20a和20b延伸到层叠芯片10的上下两面以及两个侧面。然而,外部电极20a和20b彼此隔开。
层叠芯片10具有设计为包含交替层叠的电介质层11和内部电极层12的结构。电介质层11包括用作电介质材料的陶瓷材料。内部电极层12包括贱金属材料。内部电极层12的端缘交替地露出至层叠芯片10的第一端面和层叠芯片10的不同于第一端面的第二端面。在实施方式中,第一端面与第二端面面对。外部电极20a设置在第一端面上。外部电极20b设置在第二端面上。由此,内部电极层12交替地导通至外部电极20a和外部电极20b。因此,层叠陶瓷电容器100具有多个电介质层11层叠并且每两个电介质层11夹着内部电极层12的结构。在层叠芯片10中,内部电极层12位于最外层。作为内部电极层12的层叠芯片10的上下两面被覆盖层13覆盖。覆盖层13的主要成分是陶瓷材料。例如,覆盖层13的主要成分与电介质层11的主要成分相同。
例如,层叠陶瓷电容器100可以为长度0.25mm、宽度0.125mm且高度0.125mm。层叠陶瓷电容器100可以为长度0.4mm、宽度0.2mm且高度0.2mm。层叠陶瓷电容器100可以为长度0.6mm、宽度0.3mm且高度0.3mm。层叠陶瓷电容器100可以为长度1.0mm、宽度0.5mm且高度0.5mm。层叠陶瓷电容器100可以为长度3.2mm、宽度1.6mm且高度1.6mm。层叠陶瓷电容器100可以为长度4.5mm、宽度3.2mm且高度2.5mm。然而,层叠陶瓷电容器100的尺寸并不受限制。
内部电极层12的主要成分是比如镍(Ni)、铜(Cu)、锡(Sn)等的贱金属。内部电极层12可由比如铂(Pt)、钯(Pd)、银(Ag)、金(Au)的贵金属或其合金制成。
电介质层11主要由以通式ABO3表示并具有钙钛矿结构的陶瓷材料构成。钙钛矿结构包括具有非化学计量组成的ABO3-α。例如,陶瓷材料是比如BaTiO3(钛酸钡)、CaZrO3(锆酸钙)、CaTiO3(钛酸钙)、SrTiO3(钛酸锶)、具有钙钛矿结构的Ba1-x-yCaxSryTi1-zZrzO3(0≤x≤1,0≤y≤1,0≤z≤1)。例如,电介质层11通过烧制主要成分为具有钙钛矿结构的陶瓷材料的陶瓷原料粉末而形成。
从减小层叠陶瓷电容器100的尺寸和增大层叠陶瓷电容器100的容量的角度出发,要求减小电介质层的厚度。然而,当减小电介质层11的厚度时,层叠陶瓷电容器100的寿命特性可能降低,并且层叠陶瓷电容器的可靠性可能降低。
接着,将对可靠性降低进行说明。电介质层11通过烧制主相具有通式ABO3所示的钙钛矿结构的陶瓷原料粉末并烧结陶瓷原料粉末而形成。因此,当在烧制期间将陶瓷原料粉末暴露于还原性气氛时,在陶瓷原料粉末的ABO3中产生氧缺陷。在层叠陶瓷电容器100的操作期间,电压被反复施加于电介质层11。在这种情况下,氧缺陷移动,并且势垒(barrier)可能被破坏。即,钙钛矿结构中的氧缺陷是电介质层11可靠性降低的原因之一。
因此,优选作为施主的元素包含(固溶)在钙钛矿结构的B位中。例如,作为施主的元素为比如Mo(钼)、Nb(铌)、Ta(钽)、W(钨)等。当作为施主的元素固溶在B位中时,钙钛矿结构中的氧缺陷得到抑制。因此,电介质层11的寿命延长,并且电介质层11的可靠性改善。
然而,当作为施主的元素固溶在B位中时,可能发生比如绝缘特性降低的缺陷。因此,优选作为施主的元素固溶在B位中,并且作为受主的元素也固溶在B位中。例如,作为受主的元素为Mn(锰)、Ni、Cu、Fe(铁)、Cr(铬)、Co(钴)、Zn(锌)、Y(钇)、Dy(镝)、Ho(钬)、Er(铒)等。当作为受主的元素固溶在B位中时,泄漏电流得到抑制。因此,电介质层11的绝缘特性的降低得到抑制。
然而,在这种情况下,尽管绝缘特性的降低得到抑制,但是施主效应降低。因此,在实施方式中,将说明使用能够保持施主效应和受主效应的陶瓷原料粉末的层叠陶瓷电容器100的制造方法。
在实施方式中,在具有钙钛矿结构的陶瓷原料粉末的B位中,固溶有作为施主的元素和作为受主的元素。并且,对作为施主的元素和作为受主的元素的浓度梯度进行控制。
在实施方式中,对于作为施主的元素的浓度和作为受主的元素的浓度,调节陶瓷原料粉末的外缘区域中的关系和陶瓷原料粉末的中心区域中的关系。具体地,在外缘区域中,作为施主的元素的浓度大于作为受主的元素的浓度。并且,在中心区域中,作为受主的元素的浓度大于作为施主的元素的浓度。
除了固溶在B位中的元素的浓度外,母晶体的钙钛矿结构的B位的价数(+4)与固溶在B位中的元素的价数之间的关系影响施主效应和受主效应。例如,对于作为施主的元素,当价数为+6(例如Mo)的元素的浓度与价数为+5(例如V(钒))的元素的浓度相同时,价数为+6的元素的施主效应大于价数为+5的元素的施主效应。同样地,对于作为受主的元素,当价数为+2(例如Mn)的元素的浓度与价数为+3(例如Fe)的元素的浓度相同时,价数为+2的元素的受主效应大于价数为+3的元素的受主效应。因此,从实现陶瓷原料粉末的外缘区域中作为施主的元素的浓度大于作为受主的元素的浓度并且中心区域中作为受主的元素的浓度大于作为施主的元素的浓度的角度出发,优选考虑相对于B位的价数(+4)的相对价数。
因此,在实施方式中,调节固溶在B位中的作为施主的元素的量和固溶在B位中的作为受主的元素的量,使得对于陶瓷原料粉末,满足下式(1)和下式(2)。
在中心区域中:(作为施主的元素的浓度)×(作为施主的元素的价数-4)<(作为受主的元素的浓度)×(4-作为受主的元素的价数)(1)
在外缘区域中:(作为施主的元素的浓度)×(作为施主的元素的价数-4)>(作为受主的元素的浓度)×(4-作为受主的元素的价数)(2)
当通过使用满足上述关系的陶瓷原料粉末制造层叠陶瓷电容器时,能够在陶瓷原料粉末中充分扩大外缘区域的施主效应并且能够减少氧缺陷量,其中烧制气氛/热处理气氛所引起的还原/氧化对外缘区域的施主效应影响很大。并且能够充分扩大陶瓷原料粉末的中心区域中的受主效应。并且绝缘特性得到改善。因此,能够同时实现施主效应和受主效应。因此,能够制造在寿命和绝缘特性之间良好平衡且可靠性优异的层叠陶瓷电容器。
值A为(作为施主的元素的浓度)×(作为施主的元素的价数-4)。值B为(作为受主的元素的浓度)×(4-作为受主的元素的价数)。例如,如图2A所示,在钙钛矿结构的B位中,陶瓷原料粉末具有梯度,其中值A从外缘区域到中心区域逐渐或逐步减小,并且值B具有均匀的分布而没有浓度梯度。例如,外缘区域中的作为施主的元素的浓度大于中心区域中的作为施主的元素的浓度。在图2A中,虚线示意性地表示陶瓷原料粉末的颗粒。横轴表示颗粒的位置。第一纵轴(左轴)表示值A。第二纵轴(右轴)表示值B。
陶瓷原料粉末在中心区域和外缘区域具有式(1)和式(2)的关系。因此,如图2B所示,在从外缘区域到中心区域的路径中,值A的减小的梯度可以具有局部最大值。
式(1)和式(2)的关系可应用于将两种不同的作为施主的元素添加到B位的情况。并且,式(1)和式(2)的关系可应用于将两种不同的作为受主的元素添加到B位的情况。在这些情况下,可将两种不同元素的加权均值用作作为施主的元素的浓度或作为受主的元素的浓度。
颗粒的中心区域可定义为几何重心中心区域。
将说明使作为施主的元素和作为受主的元素固溶在陶瓷原料粉末中的原因。例如,考虑通过混合陶瓷原料粉末、作为施主的元素的氧化物和作为受主的元素的氧化物,并在烧制过程中扩散每种元素,实现式(1)和式(2)的关系。然而,即使可以增大每个颗粒的外缘区域中的作为施主的元素的浓度,也难以使各种元素扩散到每个颗粒的中心区域中。因此,将作为施主的元素和作为受主的元素固溶在陶瓷原料粉末中。
接着,将说明层叠陶瓷电容器100的制造方法。图3示出层叠陶瓷电容器100的制造方法。
(原料粉末的制备工序)制备陶瓷原料粉末,其主相具有由通式ABO3表示的钙钛矿结构,并且作为施主的元素和作为受主的元素固溶在B位中,使得满足式(1)和式(2)。可以使用各种方法作为陶瓷原料粉末的合成方法。例如,可以使用固相法、溶胶-凝胶法、水热法等。例如,在Mo和Mn固溶在BaTiO3的Ti位中的情况下,固溶有Mn的BaTiO3由BaCO3、TiO2和MnCO3的混合粉末制成。之后,将Mo化合物添加到固溶有Mn的BaTiO3中。并且进行BaTiO3的颗粒生长。例如,从降低电介质层11的厚度的角度出发,优选陶瓷原料粉末的平均粒径为50nm-150nm。
根据目的,可将添加剂化合物添加到所得的陶瓷原料粉末中。添加剂化合物可以是稀土元素(Y(钇)、Sm(钐)、Eu(铕)、Gd(钆)、Tb(铽)、Dy(镝)、Ho(钬)、Er(铒)、Tm(铥)和Yb(镱))的氧化物,或者Co(钴)、Ni、Li(锂)、B(硼)、Na(钠)、K(钾)和Si(硅)的氧化物,或者玻璃。
例如,将得到的陶瓷原料粉末与添加剂进行湿混、干燥并粉碎。由此获得陶瓷材料。例如,根据需要,可通过将得到的陶瓷材料粉碎对粒径进行调整。或者,可通过将粉碎和分级进行组合来对所得陶瓷粉末的粒径进行调整。通过这些工序,获得充当电介质层的主要成分的陶瓷材料。
(层叠工序)接着,将粘合剂如聚乙烯醇缩丁醛(PVB)树脂、诸如乙醇或甲苯的有机溶剂、以及增塑剂,加入所得电介质材料并湿混。使用所得到的糊料,通过例如模涂机法或刮刀法将厚度为3-10μm的条形电介质生片涂覆在基材上,然后干燥。
然后,通过使用丝网印刷或凹版印刷来印刷用于形成内部电极的金属导电糊料,在电介质生片的表面上提供内部电极层12的图案。导电糊料包括有机粘合剂。多个图案交替地露出到一对外部电极。金属导电糊料包括作为共材的陶瓷颗粒。陶瓷颗粒的主要成分不受限制。然而,优选陶瓷颗粒的主要组分与电介质层11的主要成分相同。例如,平均粒径为50nm以下的BaTiO3可均匀地分散。
然后,将其上印刷有内部电极层图案的电介质生片冲裁成预定尺寸,并且将预定数量(例如,100至500个)的所冲裁电介质生片层叠,同时将基材剥离,使得内部电极层12和电介质层11彼此交替并且内部电极层12的端缘交替露出于电介质层11的长度方向上的两个端面,以交替地导出至一对不同极化的外部电极20a和20b。把将成为覆盖层13的覆盖片压接在层叠的电介质生片的上表面,把另一个将成为覆盖层13的覆盖片压接在层叠的电介质生片的下表面。将得到的层叠结构冲压成预定尺寸(例如1.0mm×0.5mm)。
之后,在N2气氛下从陶瓷层叠结构体中除去粘合剂。之后,从陶瓷层叠结构体的两个端面至侧面涂覆用于外部电极20a和20b的金属导电糊料,并干燥。金属导电糊料包括金属填料、共材、粘合剂、溶剂等。金属导电糊料将成为外部电极20a和20b。
(烧制工序)在250℃至500℃的温度范围的N2气氛中,将粘合剂去除。然后,在1100℃至1300℃的温度范围内在氧分压为10-5atm至10-8atm的还原气氛中将所得层叠体(compact)烧制10分钟至2小时。因此,每种化合物被烧结。以这种方式,获得陶瓷层叠结构体。
(再氧化工序)之后,可在600℃至1000℃的温度范围内在N2气氛下进行再氧化工序。通过再氧化工序,氧缺陷的浓度降低。
(外部电极的形成工序)之后,通过镀覆工序,可在外部电极20a和20b的基底层上涂覆Cu、Ni和Sn。通过该工序,制造层叠陶瓷电容器100。
在实施方式的制造方法中,使用满足式(1)和式(2)的陶瓷原料粉末。当通过使用满足上述关系的陶瓷原料粉末制造层叠陶瓷电容器时,在陶瓷原料粉末中,能够充分扩大外缘区域的施主效应并且可以减少氧缺陷量,其中烧制气氛/热处理气氛所引起的还原/氧化对外缘区域的施主效应影响很大。并且能够充分扩大陶瓷原料粉末的中心区域中的受主效应。并且绝缘特性得到改善。因此,能够实现施主效应和受主效应二者。因此,能够制造在寿命和绝缘特性之间良好平衡且可靠性优异的层叠陶瓷电容器100。
尽管已经详细说明了本发明的实施方式,但是应该理解的是,在不脱离本发明的精神和范围的情况下,可以对其进行各种改变、替换和更改。
Claims (7)
1.一种陶瓷原料粉末,其包含:
具有钙钛矿结构的主相,
其中作为施主的元素和作为受主的元素固溶在所述钙钛矿结构的B位中,
其中在所述陶瓷原料粉末的各颗粒的中心区域中,满足(所述作为施主的元素的浓度)×(所述作为施主的元素的价数-4)<(所述作为受主的元素的浓度)×(4-所述作为受主的元素的价数)的关系,
其中在所述陶瓷原料粉末的各颗粒的外缘区域中,满足(所述作为施主的元素的浓度)×(所述作为施主的元素的价数-4)>(所述作为受主的元素的浓度)×(4-所述作为受主的元素的价数)的关系。
2.如权利要求1所述的陶瓷原料粉末,其中所述钙钛矿结构的所述主相是BaTiO3。
3.如权利要求1或2所述的陶瓷原料粉末,其中所述作为施主的元素是Mo,其中所述作为受主的元素是Mn。
4.一种制造层叠陶瓷电容器的方法,其包括:
形成包括陶瓷原料粉末的生片的步骤,所述陶瓷原料粉末的主相具有钙钛矿结构;
通过交替层叠每个所述生片和每个用于内部电极的糊料,形成层叠结构的步骤;和
烧制所述层叠结构的步骤,
其中作为施主的元素和作为受主的元素固溶在所述钙钛矿结构的B位中,
其中在所述陶瓷原料粉末的各颗粒的中心区域中,满足(所述作为施主的元素的浓度)×(所述作为施主的元素的价数-4)<(所述作为受主的元素的浓度)×(4-所述作为受主的元素的价数)的关系,
其中在所述陶瓷原料粉末的各颗粒的外缘区域中,满足(所述作为施主的元素的浓度)×(所述作为施主的元素的价数-4)>(所述作为受主的元素的浓度)×(4-所述作为受主的元素的价数)的关系。
5.如权利要求4所述的方法,其中所述钙钛矿结构的所述主相是BaTiO3。
6.如权利要求4或5所述的方法,其中所述作为施主的元素是Mo,其中所述作为受主的元素是Mn。
7.一种层叠陶瓷电容器,其包括:
多个电介质层;和
多个内部电极层,
其中所述多个电介质层中的每一个和所述多个内部电极层中的每一个交替层叠,
其中所述多个电介质层通过烧制如权利要求1-3中任一项所述的陶瓷原料粉末而形成。
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