CN1849278A - 生片材用涂料、生片材、生片材的制备方法及电子部件的制备方法 - Google Patents
生片材用涂料、生片材、生片材的制备方法及电子部件的制备方法 Download PDFInfo
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Abstract
提供生片材用涂料、生片材及方法，其中所述涂料可制备生片材极薄但具有能够耐受从支持体剥离的强度、且表面平滑性优良、无针孔的生片材，适用于电子部件的薄层化和多层化。本发明提供生片材用涂料，其含有陶瓷粉末、以缩丁醛系树脂为主成分的粘合剂树脂、和溶剂。上述溶剂含有将对粘合剂树脂的溶解性参数数值化的SP值为10以上的第1溶剂、和上述SP值为8以上但不足10的第2溶剂。上述涂料中，相对于溶剂的总质量100质量％，含有20～60质量％、优选25～60质量％的第2溶剂。
Description
技术领域
本发明涉及生片材用涂料、生片材、生片材的制备方法及电子部件的制备方法，更详细地说，涉及涂料、生片材及方法，其中所述涂料可制备生片材极薄但表面平滑性优良、无针孔的生片材，适用于电子部件的薄层化和多层化。
背景技术
近年来，随着各种电器的小型化，装在电器内部的电子部件的小型化和高性能化不断推进。作为电子部件之一，有CR内置型基板、多层陶瓷电容器等陶瓷电子部件，该陶瓷电子部件也在谋求小型化和高性能化。
为了推进这种陶瓷电子部件的小型化和高容量化，强烈要求电介质层的薄层化。最近，构成电介质层的电介质生片材的厚度达到数μm以下。
为了制备陶瓷生片材，通常首先准备由陶瓷粉体、粘合剂(丙烯酸系树脂、缩丁醛系树脂等)、增塑剂(邻苯二甲酸酯类、二醇类、己二酸、磷酸酯类)和有机溶剂(甲苯、MEK、丙酮等)构成的陶瓷涂料。然后，使用刮板法等将该陶瓷涂料涂布在载体片材(PET、PP制的支持体)上，加热干燥来制备。
另外，近年来正在探讨准备在溶剂中混合有陶瓷粉体和粘合剂的陶瓷混悬液，将该混悬液挤压成形得到薄膜状成形体，双轴拉伸该成形体进行制备。
具体地说明使用上述陶瓷生片材制备多层陶瓷电容器的方法，是在陶瓷生片材上，以规定图案印刷含有金属粉体和粘合剂的内部电极用导电性糊料，使之干燥来形成内部电极图案。之后，由载体片材剥离生片材，层压其至所希望的层数。在此，考察了在层压前由载体片材剥离生片材的方法、与在层压压合后剥离载体片材的两种方法，但没有大的区别。最后，将该层压体切成片状制成生片。烧结这些生片后，形成外部电极，制备多层陶瓷电容器等电子部件。
制备多层陶瓷电容器时，基于电容器所需的期望的静电电容，形成有内部电极的片材的层间厚度在约3μm～100μm左右的范围内。另外，在多层陶瓷电容器中，形成了电容器芯片层压方向的外侧部分上未形成内部电极的部分。
一般随着使生片材的厚度变薄，片材的表面平滑性降低，层压困难，这是个课题。
近年来，随着电器的小型化，急速进行着其中使用的电子部件的小型化。在以多层陶瓷电容器为代表的多层电子部件中，急速进行着层压数的增加、层间厚度的薄层化。为了应对这种技术动向，决定层间厚度的生片材厚度正在由3μm以下变成2μm以下。为此，在多层陶瓷电容器的制备工序中，需要处理极薄的生片材，需要设计非常高的生片材物性。
作为这种极薄生片材的物性所要求的特性，可列举出片材强度、可挠性、平滑性、层压时的接合性、处理性(静电性)等，还要求高量纲下的平衡。
特别是片材变薄时，无法忽视厚度对片材表面的粗糙度(凹凸)的影响。也就是说，厚片材中无需考虑的表面状态的变化在薄层片材中随着片材厚度本身的变化而变化。表面粗糙的凹部在烧结时对外加电压不耐受，会导致短路。为此，制备表面平滑(＝表面粗糙度的变化小)且厚度均匀的片材，在多层片式电容器的制备上是不可缺少的关键技术。
应说明的是，如下面专利文献1所示，已知在含有水性溶剂的生片材用浆料中，为了消除短路缺陷，将聚合度1000以上的聚乙烯醇缩丁醛树脂用作粘合剂的技术。
但是，专利文献1中，特别是不但没有想要使有机溶剂系生片材薄层化，同时随着生片材厚度的变薄，表面平坦性下降，难于层压，这是个课题。
专利文献2中，公开了为了加速蒸发速度提高片材的表面性使用蒸发速度快的溶剂的技术。但是，加速蒸发速度的方法虽然对获得厚片材有效，但在使片材变薄时却有使表面性变差的副作用。
如下述专利文献3所述，已知在水性涂料中规定了片材的调和组成比、脱泡条件、干燥温度条件的发明。
但是，在该技术中，由于组成的限制可能无法得到所希望物性的片材，另外加入脱泡工序使工序变得繁杂。
如下述专利文献4所述，已知轧制片材欲改善表面性的技术。
但是，在该技术中，当薄层化生片材时，由于加压可能损坏片材。
专利文献1：特开平6-206756号公报
专利文献2：特许公报第2866137号
专利文献3：特开2000-335971号公报
专利文献4：特开2001-114568号公报
发明内容
发明所要解决的课题
本发明的目的在于提供生片材用涂料、生片材及方法，其中其中所述涂料可制备生片材极薄但具有能够耐受从支持体剥离的强度、且表面平滑性优良、无针孔的生片材，适用于电子部件的薄层化和多层化。
解决课题的方法
为了达成上述目的，本发明涉及的生片材用涂料含有陶瓷粉末、以缩丁醛系树脂为主成分的粘合剂树脂、和溶剂，其特征在于，
上述溶剂含有作为溶解性参数的SP值为10以上的第1溶剂、和上述SP值为8以上但不足10的第2溶剂，
相对于上述溶剂的总质量100质量％，含有20～60质量％、优选25～60质量％的第2溶剂。
使用缩丁醛系树脂的涂料组成，考虑到树脂在溶剂中的溶解性问题，以高极性的醇为主成分。对此，本发明涉及的涂料中使用的分散剂显示了高于第2溶剂的溶解性。因此，通过调整溶剂的极性以使涂料内不发生颜料的凝集，可提高颜料的分散，制备表面性优良的片材。
即，通过使涂料中的溶剂成分成为极性范围大的构成，可兼顾树脂的溶解性和分散剂的溶解性。结果，树脂·颜料均成为分散性良好的涂料，片材化时表面变得平滑。另外，片材表面粗糙度降低至与层间厚度相比非常小，因此可减小层间厚度(薄层化)，可进一步多层化·小型化电子部件。
例如，可将烧结后的电介质层(烧结后的生片材)的厚度薄层化至5μm以下、优选3μm以下、进一步优选2μm以下。另外也可增加层压数。而且可减少短路等缺陷。
优选上述溶剂中第2溶剂相对于第1溶剂的质量比为0.2～2.0，进一步优选为0.5～1.5。
第2溶剂的质量比过小，则由于分散剂在溶剂中的溶解性降低等，表面平滑性降低，质量比过大，则由于树脂在溶剂中的溶解性降低等，表面平滑性降低。
本发明的涂料优选进一步含有分散剂，上述分散剂为聚乙二醇系阴离子分散剂。另外，分散剂的SP值优选为8～9。这种分散剂对第2溶剂的溶解性好，结果可提高分散性。
优选上述第1溶剂为醇类，上述第2溶剂含有酮类、酯类、芳香族类中的至少一种。这种情况下，优选上述第1溶剂为选自甲醇、乙醇、丙醇、丁醇中的至少一种，上述第2溶剂含有选自甲乙酮、甲基异丁基酮、乙酸乙酯、乙酸丁酯、甲苯、二甲苯中的至少一种。
优选上述缩丁醛树脂为聚缩丁醛树脂，上述聚缩丁醛树脂的聚合度为1000以上1700以下，树脂的缩丁醛化度大于64％小于78％，残留乙酰基量不足6％。
聚缩丁醛树脂的聚合度过小，例如薄层化至5μm以下、优选3μm以下左右时，有难于得到充分的机械强度的倾向。聚合度过大，则有片材化时的表面粗糙度劣化的倾向。聚缩丁醛树脂的缩丁醛化度过低，则有在涂料中的溶解性劣化的倾向，过高则有片材表面粗糙度劣化的倾向。残留的乙酰基量过多，则有片材表面粗糙度劣化的倾向。
优选相对于上述陶瓷粉体100质量份含有5质量份以上6.5质量份以下的上述粘合剂树脂。粘合剂树脂的含量过少，则有片材强度降低，同时叠层性(层压时的接合性)劣化的倾向。粘合剂树脂的含量过多，则有发生粘合剂树脂的偏析分散性变差的倾向，以及片材表面粗糙度劣化的倾向。
优选上述陶瓷粉体的粒径为0.01～0.5μm。通过细化粉体的粒径，使生片材薄层化。另外，优选生片材用涂料中的不挥发成分为10～48质量％。作为不挥发成分，可列举出陶瓷粉体、粘合剂、增塑剂、分散剂等。
本发明涉及的生片材的制备方法包括：
准备上述生片材用涂料的工序，和
使用上述生片材用涂料成形陶瓷生片材的工序。
本发明涉及的陶瓷电子部件的制备方法包括：
准备上述生片材用涂料的工序，
使用上述生片材用涂料成形陶瓷生片材的工序，
使上述生片材干燥的工序，
通过内部电极层层压干燥后的生片材，得到生片的工序，和
烧结上述生片的工序。
使用上述生片材用涂料制备本发明涉及的生片材。
根据本发明，可提供涂料、生片材及方法，其中所述涂料可制备生片材极薄但具有能够耐受从支持体剥离的强度、且表面平滑性优良、无针孔的生片材，适用于电子部件的薄层化和多层化。
附图说明
[图1]图1为本发明的一个实施方式涉及的多层陶瓷电容器的简略剖面图。
[图2]图2为显示图1所示的多层陶瓷电容器的制备过程的要部剖面图。
具体实施方式
下面基于附图所示的实施方式说明本发明。
首先，作为使用本发明涉及的生片材用涂料(电介质糊料)和生片材制备的电子部件的一个实施方式，对多层陶瓷电容器的整体构成进行说明。
如图1所示，本实施方式涉及的多层陶瓷电容器2具有电容器基体4、第1端子电极和第2端子电极8。电容器基体4具有电介质层10、和内部电极层12，在电介质层10之间，交互层压有这些内部电极层12。交互层压的一个内部电极层12对电容器基体4的一个端部上形成的第1端子电极6的内侧电连接。而交互层压的另一个内部电极层12对电容器基体4的另一个端部上形成的第2端子电极8的内侧电连接。
电介质层10的材质无特别限定，例如可由钛酸钙、钛酸锶和/或钛酸钡等电介质材料构成。各电介质层10的厚度无特别限定，一般为数μm～数百μm。特别是本实施方式中，优选薄层化至5μm以下，更优选3μm以下。
端子电极6和8的材质也无特别限定，通常使用铜或铜合金、镍或镍合金等，也可使用银或银与钯的合金等。端子电极6和8的厚度无特别限定，通常为10～50μm左右。
多层陶瓷电容器2的形状和尺寸可根据目的和用途适当决定。多层陶瓷电容器2为长方体形时，通常为长(0.6～5.6mm，优选0.6～3.2mm)×宽(0.3～5.0mm，优选0.3～1.6mm)×高(0.1～1.9mm，优选0.3～1.6mm)左右。
下面，说明本实施方式涉及的多层陶瓷电容器2的制备方法的一个例子。
(1)首先，为了制备烧结后构成图1所示的电介质层10的陶瓷生片材，准备电介质涂料(生片材用涂料)。
电介质涂料由混炼电介质原料(陶瓷粉末)和有机载体得到的有机溶剂系涂料构成。
作为电介质原料，可从由复合氧化物和氧化物构成的各种化合物、例如碳酸盐、硝酸盐、氢氧化物、有机金属化合物等中适当选择，混合使用。电介质原料作为通常平均粒径为0.1～3μm、优选0.4μm以下的粉体来使用。应说明的是，为了形成极薄的生片材，希望使用薄于生片材厚度的细小粉体。
有机载体是指在有机溶剂中溶解了粘合剂树脂的物质。作为有机载体所用的粘含剂树脂，在本实施方式中，可使用聚乙烯醇缩丁醛树脂。该聚缩丁醛树脂的聚合度为1000以上1700以下，树脂的缩丁醛化度大于64％小于78％，优选大于64％小于等于70％，其残留乙酰基量不足6％，优选为3％以下。
聚缩丁醛树脂的聚合度例如可由作为原料的聚乙烯醇缩醛树脂的聚合度来测定。缩丁醛化度例如可根据JISK6728来测定。残留乙酰基量可根据JISK6728来测定。
聚缩丁醛树脂的聚合度过小，例如薄层化至5μm以下、优选3μm以下左右时，有难于得到充分的机械强度的倾向。聚合度过大，则有片材化时的表面粗糙度劣化的倾向。聚缩丁醛树脂的缩丁醛化度过低，则有在涂料中的溶解性劣化的倾向，过高则有片材表面粗糙度劣化的倾向。残留的乙酰基量过多，则有片材表面粗糙度劣化的倾向。
在本实施方式中，有机载体所使用的有机溶剂含有溶解性参数SP值为10以上的第1溶剂、和上述SP值为8以上但不足10的第2溶剂。在本发明中，SP值为对于溶剂的蒸发热ΔH[cal/mol]、气体常数R[cal/K·mol]、温度T[K]、分子量n[g/mol]、密度ρ[g/cm3]，根据((ΔH-RT)·ρ/n)1/2定义的数值。
第1溶剂可列举出甲醇、乙醇、丙醇、丁醇等醇类。另外，第2溶剂可列举出酮类、酯类、芳香族类，酮类优选使用甲乙酮、甲基异丁基酮，酯类可列举出乙酸乙酯、乙酸丁酯，芳香族类可列举出甲苯、二甲苯等。
相对于溶剂的总质量100质量％，含有20～60质量％、优选25～60质量％的第2溶剂。溶剂中第2溶剂相对于第1溶剂的质量比优选为0.2～2.0，进一步优选为0.5～1.5。
优选事先将粘合剂树脂溶解于醇系溶剂，过滤制成溶液，在该溶液中添加电介质粉体及其他成分。高聚合度的粘合剂树脂难溶于溶剂，在通常的方法中，有涂料的分散性恶化的倾向。在本实施方式的方法中，在上述良溶剂中溶解高聚合度的粘合剂树脂后，在该溶液中添加陶瓷粉体及其他成分，因此可改善涂料分散性，可抑制未溶解树脂的产生。应说明的是，利用上述溶剂以外的溶剂，无法提高固形分浓度，同时有增大清漆粘度的经时变化的倾向。
在电介质涂料中，根据需要可含有选自各种分散剂、增塑剂、除静电剂、电介质、玻璃料、绝缘体等中的添加物。
在本实施方式中，作为分散剂无特别限定，优选使用聚乙二醇系非离子性分散剂，其亲水性·亲油性平衡(HLB)值为5～6。分散剂的SP值为8～9。相对于陶瓷粉体100质量份，添加有优选0.5质量份以上1.5质量份以下、进一步优选0.5质量份以上1.0质量份以下的分散剂。
HLB超出上述范围，则有涂料粘度增大的同时片材表面粗糙度增大的倾向。当分散剂不是聚乙二醇系的非离子性分散剂时，涂料粘度增大，同时片材表面粗糙度增大，或生片伸长度降低，因此非优选。
分散剂的添加量过少，则片材表面粗糙度有增大的倾向，过多则有片材拉伸强度和叠层性降低的倾向。
在本实施方式中，作为增塑剂，优选使用邻苯二甲酸二辛酯，相对于粘合剂树脂100质量份，优选含有增塑剂40质量份以上70质量份以下，进一步优选40～60质量份。与其他增塑剂相比，邻苯二甲酸二辛酯由于兼有片材强度和片材伸展度，因此优选，由于由支持体的剥离强度小，易剥离，因此特别优选。应说明的是，该增塑剂的含量过少，则有片材伸展度小、可挠性小的倾向。而含量过多，则有增塑剂从片材中渗出，易发生增塑剂对片材的偏析，片材的分散性降低的倾向。
在本实施方式中，相对于电介质粉体100质量份，电介质涂料中含有1质量份以上6质量份以上、优选1～3质量份的水。水含量过少，则吸湿引起的涂料特性的经时变化增大，变得优选的同时，涂料粘度有增大的倾向，涂料的过滤特性有劣化的倾向。水含量过多，则发生涂料的分离或沉降，分散性变差，片材的表面粗糙度有劣化的倾向。
在本实施方式中，相对于电介质粉体100质量份，优选添加3质量份以上15质量份以下、进一步优选5～10质量份的烃系溶剂、工业用汽油、煤油、溶剂石脑油中的至少一种。通过添加这些添加物，可提高片材强度和片材表面粗糙度。这些添加物的添加量过少，则添加效果少，添加量过多，则相反有片材强度和片材表面粗糙度劣化的倾向。
相对于电介质粉体100质量份，优选含有5质量份以上6.5质量份以下的粘合剂树脂。粘合剂树脂的含量过少，则有片材强度降低的同时叠层性(层压时的接合性)劣化的倾向。粘合剂树脂的含量过多，则有发生粘合剂树脂的偏析、分散性恶化的倾向，有片材表面粗糙度劣化的倾向。
以陶瓷粉体和粘合剂树脂和增塑剂的总体积为100体积％时，电介体粉体所占的体积比例优选为62.42％以上72.69％以下，进一步优选63.93％以上72.69以下％。该体积比例过小，则有易发生粘合剂的偏析、分散性恶化的倾向，有表面粗糙度劣化的倾向。体积比例过大，则片材强度降低的同时，有叠层性恶化的倾向。
在本实施方式中，电介质涂料中优选含有除静电剂，该除静电剂优选为咪唑啉系除静电剂。除静电剂为咪唑啉系除静电剂以外时，除静电效果小的同时，有片材强度、片材伸展度或接合性劣化的倾向。
相对于陶瓷粉体100质量份，含有0.1质量份以上0.75质量份以下、进一步优选0.25～0.5质量份的除静电剂。除静电剂的添加量过少，则除静电效果小，过多则片材的表面粗糙度劣化的同时，片材强度有劣化的倾向。除静电效果过小，则在从陶瓷生片材上剥离作为支持体的载体片材时等易产生静电，易发生生片材上出现褶皱等不良。
使用该电介质涂料，利用刮板法等，如图2所示，在作为支持体的载体片材30上，以优选0.5～30μm、更优选0.5～10μm左右的厚度，形成生片材10a。在载体片材30形成后，干燥生片材10a。
生片材的干燥温度优选为50～100℃，干燥时间优选为1～20分钟。干燥后的生片材厚度与干燥前相比收缩至5～25％。干燥后的生片材10a的厚度优选为3μm以下。
(2)如图2所示，准备上述载体片材30和另外的载体片材20，在之上形成剥离层22，在之上形成规定图案的电极层12a，在其前后，在未形成该电极层12a的剥离层22的表面，形成与电极层12a厚度基本相同的空白图案层24。
作为载体片材20、30，例如使用PET薄膜等，为了改善剥离性，优选涂布有硅等。这些载体片材20、30的厚度无特别限定，优选为5～100μm。
剥离层22优选含有与构成生片材10a的电介质相同的电介质粒子。该剥离层22除了电介质粒子以外还含有粘合剂、增塑剂和脱模剂。电介质粒子的粒径可与生片材所含的电介质粒子的粒径相同，优选更小。
在本实施方式中，剥离层22的厚度优选小于等于电极层12a的厚度，优选设定为60％以下的厚度、进一步优选30％以下。
作为剥离层22的涂布方法，无特别限定，由于有必要形成得极薄，优选例如使用线棒涂布器或模涂器的涂布方法。应说明的是，剥离层22的厚度的调整可通过选择不同线径的线棒涂布器来进行。即，为了使剥离层22的涂布厚度变薄，可选择线径小的线棒涂布器，相反为了形成得较厚，可选择粗线径的线棒涂布器。在涂布后干燥剥离层22。干燥温度优选为50～100℃，干燥时间优选为1～10分钟。
作为用于剥离层22的粘合剂，例如由丙烯酸树脂、聚乙烯醇缩丁醛树脂、聚乙烯醇缩醛、聚乙烯醇、聚烯烃、聚氨酯、聚苯乙烯、或由这些共聚物构成的有机质、或乳液构成。剥离层22所含的粘合剂可与生片材10a所含的粘合剂相同也可不同，优选相同。
作为用于剥离层22的增塑剂，无特别限定，可列举出例如邻苯二甲酸酯类、邻苯二甲酸二辛酯、己二酸、磷酸酯、二醇类等。剥离层22所含的增塑剂可与生片材10a所含的增塑剂相同也可不同。
作为用于剥离层22的剥离剂，无特别限定，可列举出例如石蜡、蜡、硅油等。剥离层22所含的剥离剂可与生片材所含的剥离剂相同也可不同。
在剥离层22中，相对于电介质粒子100质量份，优选以2.5～200质量份、进一步优选5～30质量份、特别优选8～30质量份左右含有粘合剂。
在剥离层22中，相对于粘合剂100质量份，以0～200质量份、优选20～200质量份、进一步优选50～100质量份含有增塑剂。
在剥离层22中，相对于粘合剂100质量份，以0～100质量份、优选2～50质量份、进一步优选5～20质量份含有剥离剂。
在载体片材的表面形成剥离层22后，在剥离层22的表面以规定图案形成在烧结后构成内部电极层12的电极层12a。电极层12a的厚度优选为0.1～2μm、更优选为0.1～1.0μm左右。电极层12a可以以单一的层构成，或者也可以以2以上的组成不同的多个层构成。
通过例如使用电极涂料的印刷法等厚膜形成方法、或蒸镀、溅射等薄膜法，可在剥离层22的表面形成电极层12a。通过作为厚膜法的1种的丝网印刷法或凹版印刷法，在剥离层22的表面形成电极层12a时，如下操作。
首先，准备电极涂料。混炼各种导电性金属或由合金构成的导电体材料、或者烧结后成为上述导电体材料的各种氧化物、有机金属化合物、或树脂酸盐等和有机载体，调制电极涂料。
作为制备电极涂料时使用的导体材料，使用Ni或Ni合金甚至他们的混合物。这些导体材料为球状、鳞片状等，其形状无特别限定，也可为混合这些形状的材料而成的材料。导体材料的平均粒径通常可以为0.1～2μm、优选0.2～1μm左右。
有机载体含有粘合剂和溶剂。粘合剂可列举出例如乙基纤维素、丙烯酸树脂、聚乙烯醇缩丁醛、聚乙烯醇缩醛、聚乙烯醇、聚烯烃、聚氨酯、聚苯乙烯、或他们的共聚物等，特别优选聚乙烯醇缩丁醛等缩丁醛系。
电极涂料中，相对于导体材料(金属粉体)100质量份，优选含有8～20质量份的粘合剂。溶剂可使用例如萜品醇、丁基卡比醇、煤油等公知的物质中的任一种。相对于所有涂料，溶剂含量优选为20～55质量％左右。
为了改善接合性，在电极涂料中优选含有增塑剂。增塑剂可列举出邻苯二甲酸苄丁酯(BBP)等邻苯二甲酸酯、己二酸、磷酸酯、二醇类等。在电极涂料中，相对于粘合剂100质量份，增塑剂优选为10～300质量份，进一步优选为10～200质量份。应说明的是，增塑剂或粘合剂的添加量过多，则电极层12a的强度有显著降低的倾向。另外，为了提高电极层12a的转印性，优选在电极涂料中添加增塑剂和/或粘合剂，提高电极涂料的接合性和/或粘合性。
以印刷法在剥离层22的表面上形成规定图案的电极涂料层后、或之前，在未形成电极层12a的剥离层22的表面上形成基本与电极层12a相同厚度的空白图案层24。空白图案层24由与生片材相同的材质构成，通过相同的方法形成。根据需要干燥电极层12a和空白图案层22。干燥温度无特别限定，优选为70～120℃，干燥时间优选为5～15分钟。
(3)之后，在生片材10a的表面接合电极层12a。为此，在生片材10a的表面与载体片材20一起推压电极层12a和空白图案层24，加热加压，在生片材10a的表面转印电极层12a和空白图案层24。但是，从生片材侧来看，生片材10a转印在电极层12a和空白图案层24上。
该转印时的加热和加压，可利用冲压进行加压·加热，利用压光辊进行加压·加热，优选利用一对辊进行。其加热温度和加压力无特别限定。
如果在单一的生片材10a上层压形成有单一层的规定图案的电极层12a的生片材，可得到交互层压多个电极层12a和生片材10a的层压块。之后，在此层压体下面，层压外层用的生片材(层压有多层未形成电极层的生片材的较厚层压体)。之后，在层压体上侧，同样地形成外层用生片材后，进行最终加压。
最终加压的压力优选为10～200Mpa。加热温度优选为40～100℃。之后，将层压体切为规定大小，形成生片。该生片进行脱粘合剂处理、烧结处理，然后为了再氧化电介质层，进行热处理。
脱粘合剂处理可在通常的条件下进行，但在内部电极层的导电体材料中使用Ni或Ni合金等的贱金属时，特别优选在下述条件下进行。
升温速度：5～300℃/小时，
保持温度：200～400℃，
保持时间：0.5～20小时，
环境：加湿的N2和H2的混合气体。
烧结条件优选下述条件。
升温速度：50～500℃/小时，
保持温度：1100～1300℃，
保持时间：0.5～8小时，
冷却速度：50～500℃/小时，
环境气体：加湿的N2和H2的混合气体。
但是，烧结时的空气环境中的氧分压优选在10-2Pa以下。超出上述范围，则内部电极层有氧化的倾向，氧分压过低，则内部电极层的电极材料有发生异常烧结、断裂的倾向。
进行了这种烧结后的热处理，优选在保持温度或最高温度1000℃以上、进一步优选1000～1100℃下进行。热处理时的保持温度或最高温度不足上述范围时电介质材料的氧化不充分，因此有绝缘电阻寿命变短的倾向，若超出上述范围，则不仅内部电极的Ni氧化、容量下降，还有与电介质基体反应、寿命也缩短的倾向。热处理时的氧分压高于烧结时的还原环境，优选为10-3～1Pa，更优选为10-2～1Pa。不足上述范围，则电介质层2a的再氧化困难，超过上述范围则内部电极层3有氧化的倾向。其他的热处理条件优选下述条件。
保持时间：0～6小时，
冷却速度：50～500℃/小时，
环境用气体：加湿的N2气等。
应说明的是，加湿N2气或混合气体可使用例如加湿器等。此时，水温为0～75℃左右。另外，脱粘合剂处理、烧结和热处理可各自连续进行，也可独立进行。连续进行时，优选脱粘合剂处理后，不冷却，改变环境，接着升温至烧结时的保持温度进行烧结，然后冷却，达到热处理的保持温度时改变环境进行热处理。另一方面，独立进行时，优选在烧结时在N2气或加湿的N2气环境下升温至脱粘合剂处理时的保持温度，之后改变环境进一步继续升温，冷却至热处理时的保持温度后，优选再次改变为N2气或加湿的N2气环境继续冷却。热处理时，N2气环境下升温至保持温度后，可改变环境，也可在加湿的N2气环境下进行热处理的全过程。
对这样得到的烧结体(元件主体4)，例如用滚磨、喷砂等实施端面研磨，烧结端子电极用涂料形成端子电极6、8。端子电极用涂料的烧结条件优选例如在加湿的N2和H2的混合气体中600～800℃下进行10分钟～1小时左右。然后，根据需要通过在端子电极6、8上电镀等形成焊盘层。应说明的是，可与上述电极涂料相同地调制端子电极用涂料。
这样制备的本发明的多层陶瓷电容器通过焊接等装在印刷基板上等，用于各种电器等。
利用使用本实施方式涉及的电介质涂料(生片材用涂料)和生片材的多层陶瓷电容器的制备方法，可制备即使生片材极薄也具有能够耐受从支持体剥离的强度、且表面平滑性优良、无针孔的生片材。例如，可将烧结后的电介质层(烧结后的生片材)的厚度薄层化至5μm以下，优选3μm以下，进一步优选2μm以下。还可增大层压数。而且可减少短路等缺陷。
在使用本实施方式涉及的电介质涂料(生片材用涂料)和生片材的多层陶瓷电容器的制备方法中，使用特定种类的、HLB在特定范围的分散剂。为此，即使为例如5μm以下左右的极薄的生片材，也具有能够耐受从支持体剥离的强度，且具有良好的接合性和处理性。另外，片材的表面粗糙度也小，且叠层性优良。为此，易于通过电极层层压多个生片材。
在使用本实施方式涉及的电介质涂料(生片材用涂料)和生片材的多层陶瓷电容器的制备方法中，电介质涂料含有除静电剂，此除静电剂为咪唑啉系除静电剂。为此，可制备即使为例如5μm以下左右的极薄的生片材也具有能够耐受从作为支持体的载体片材剥离的强度、抑制从载体片材的剥离时等产生的静电、且具有良好的接合性和处理性的生片材。另外，片材的表面粗糙度也小，且叠层性优良。为此，易于通过电极层层压多个生片材。
在本实施方式涉及的多层陶瓷电容器的制造方法中，生片材不会破坏或变形，可容易且高精度地在生片材的表面上转印高精度干式电极层。
应说明的是，本发明不限于上述实施方式，可在本发明的范围内进行各种变化。
例如，本发明的方法不限于多层陶瓷电容器的制备方法，也可作为其他的层压型电子部件的制备方法来应用。
实施例
下面，基于更详细的实施例来说明本发明，但本发明并不限于这些实施例。
实施例1
生片材用涂料的制备
作为陶瓷粉体的起始原料，使用BaTiO3粉体(BT-02堺化学工业(株)。准备陶瓷粉体副成分添加物，以使相对于该BaTiO3粉体100质量份，(Ba0.6Ca0.4)SiO3为1.48质量份，Y2O3为1.01质量份，MgCO3为0.72质量％，Cr2O3为0.13质量％，和V2O5为0.045质量％。
最初用球磨机仅混合副成分添加物，浆料化。即，用球磨机对副成分添加物(总量8.8g)、乙醇∶正丙醇∶二甲苯＝42.5∶42.5∶15的溶剂15g、分散剂(0.1g)和粘合剂(副成分添加物的2质量％(作为清漆添加量为1.1g))，进行20小时的予粉碎，得到予粉碎浆料。
然后，相对于BaTiO3 191.2g，用球磨机混合副成分添加物的予粉碎浆料24g、乙醇123g、正丙醇123g、二甲苯56g、甲乙酮136g、矿油精15g、分散剂1.4g、DOP(邻苯二甲酸二辛酯)6g、咪唑啉系除静电剂0.8g、BH-6的清漆(以乙醇/正丙醇＝1∶1溶解积水化学公司制聚乙烯醇缩丁醛树脂BH-6)80g 20小时，得到陶瓷涂料(生片材用涂料)。
应说明的是，作为分散剂，使用聚乙二醇系的非离子性分散剂(HLB＝5～6)。分散剂的SP值为8～9。作为粘合剂，添加积水化学公司制BH6(聚缩丁醛树脂/PVB)的15％清漆(以乙醇/正丙醇＝1∶1溶解积水化学公司制BH-6)作为固形份。
该陶瓷涂料中的溶剂成分由乙醇和正丙醇构成的第1溶剂、和甲乙酮和二甲苯构成的第2溶剂构成。相对于100质量％所有溶剂，该溶剂中第2溶剂的质量比例为36质量％。应说明的是，甲乙酮的SP值如表1所示，为9.3。表1一并示出了聚乙烯醇缩丁醛树脂(PVB)中的溶解性和分散剂中的溶解性。表1中，○表示溶解性优良，×表示不溶性。
作为粘合剂树脂的聚缩丁醛树脂的聚合度为1400，其缩丁醛化度为69％±3％，残留乙酰基量为3±2％。在陶瓷涂料中，相对于陶瓷粉体(含有陶瓷粉体副成分的添加物)100质量份，以6质量份含有该粘合剂树脂。以陶瓷涂料中的陶瓷粉体、粘合剂树脂和增塑剂的总体积为100体积％时，陶瓷粉体所占的体积比例为67.31体积％。
相对于粘合剂树脂100质量份，在陶瓷涂料中以50质量份含有作为增塑剂的DOP。相对于陶瓷粉体100质量份，含有2质量份水。相对于陶瓷粉体100质量份，含有0.7质量份作为分散剂的聚乙二醇系非离子性分散剂。
在涂料中，相对于陶瓷粉体100质量份，添加5质量份烃系溶剂、工业用汽油、煤油、溶剂石脑油中的至少一种的矿油精。
涂料的粘度为180mPa·s。使用B型粘度计，使用S21作为转子，测定时的温度为25℃，在滴出涂料后立即测定涂料的粘度。测定转数为50rpm。
生片材的制备
利用线棒涂布器在作为支持体薄膜的PET薄膜上涂布上述得到的涂料，通过干燥制备厚度为1μm的生片材。涂布速度为50m/min，干燥条件为干燥炉内的温度为60℃～70℃，干燥时间为2分钟。
生片材的评价
之后，测定生片材的光泽度。光泽度是利用日本电色工业株式会社制VGS-1D，基于JIS Z-8741(1983)方法3测定生片材的表面光泽度。光泽度的％越大，表面平滑性越好。结果示于表2。在光泽度的测定中，将70％以上判断为良好(○)，将其余判断为不良(×)。
[表1]
| 溶剂种类 | SP值 | 溶解性 | |||
| PVB | 分散剂 | ||||
| 醇 | 比较例1 | 乙醇 | 12.9 | ○ | × |
| 比较例2 | 1-丙醇 | 11.9 | ○ | × | |
| 酮 | 实施例1 | 甲乙酮 | 9.3 | ○ | ○ |
| 实施例2 | 甲基异丁基酮 | 8.4 | × | ○ | |
| 酯 | 实施例3 | 乙酸乙酯 | 9.1 | × | ○ |
| 实施例4 | 乙酸正丁酯 | 8.6 | × | ○ | |
| 芳香族 | 实施例5 | 甲苯 | 8.9 | 溶涨 | ○ |
| 实施例6 | 二甲苯 | 8.9 | 溶涨 | ○ | |
| 比较例3 | 正庚醇 | 7.5 | × | ○ | |
[表2]
| 溶剂种类 | SP量 | 第2溶剂/总溶剂比 | 光泽度 | 判定 | ||
| [wt％] | [％] | |||||
| 醇 | 比较例1 | 乙醇 | 12.9 | 12 | 58 | × |
| 比较例2 | 1-丙醇 | 11.9 | 12 | 60 | × | |
| 酮 | 实施例1 | 甲乙酮 | 9.3 | 36 | 73 | ○ |
| 实施例2 | 甲基异丁基酮 | 8.4 | 36 | 65 | ○ | |
| 酯 | 实施例3 | 乙酸乙酯 | 9.1 | 36 | 70 | ○ |
| 实施例4 | 乙酸正丁酯 | 8.6 | 36 | 69 | ○ | |
| 芳香族 | 实施例5 | 甲苯 | 8.9 | 36 | 74 | ○ |
| 实施例6 | 二甲苯 | 8.9 | 36 | 70 | ○ | |
| 比较例3 | 正庚醇 | 7.5 | 12 | 50 | × |
[表3]
| 中极性溶剂种类 | 第2溶剂/总溶剂比 | 第2溶剂/第1溶剂比 | 光泽度 | 判定 | |
| [wt％] | [-] | [％] | |||
| 比较例4 | 二甲苯 | 15 | 0.18 | 50 | × |
| 实施例6 | 二甲苯 | 36 | 0.56 | 70 | ○ |
| 实施例7 | 二甲苯 | 58 | 1.46 | 65 | ○ |
| 比较例5 | 二甲苯 | 66 | 2.14 | 55 | × |
实施例2
除代替甲乙酮使用甲基异丁基酮之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
实施例3
除代替甲乙酮使用乙酸乙酯之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
实施例4
除代替甲乙酮使用乙酸正丁酯之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
实施例5
除代替甲乙酮使用甲苯之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
实施例6
除代替甲乙酮使用二甲苯之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。应说明的是，溶剂中第2溶剂与第1溶剂1的质量比如表3所示，为0.59。
比较例1
除代替甲乙酮使用乙醇、使第2溶剂的质量比相对于所有溶剂100质量％为11质量％之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
比较例2
除代替甲乙酮使用1-丙醇、使第2溶剂的质量比相对于所有溶剂100质量％为11质量％之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
比较例3
除代替甲乙酮使用正庚醇、使第2溶剂的质量比相对于所有溶剂100质量％为11质量％之外，与实施例1一样，制备生片材，进行同样的评价。结果见表2。
实施例7
除相对于溶剂的总质量100质量％含有58质量％的第2溶剂、使溶剂中第2溶剂相对于第1溶剂的质量比为1.46之外，与实施例6一样，制备生片材，进行同样的评价。结果见表3。
比较例4
除相对于溶剂的总质量100质量％含有15质量％的第2溶剂、使溶剂中第2溶剂相对于第1溶剂的质量比为0.18之外，与实施例6一样，制备生片材，进行同样的评价。结果见表3。
比较例5
除相对于溶剂的总质量100质量％含有66质量％的第2溶剂、使溶剂中第2溶剂相对于第1溶剂的质量比为2.14之外，与实施例6一样，制备生片材，进行同样的评价。结果见表3。
评价
如表2和3所示，可确认相对于溶剂的总质量100质量％，含有20～60质量％、优选25～60质量％的第2溶剂，溶剂中第2溶剂相对于第1溶剂的质量比为0.2～2.0、优选0.5～1.5时，光泽度提高，生片材表面的平滑性提高。
Claims (13)
1.一种生片材涂料，其为含有陶瓷粉体、以缩丁醛系树脂为主成分的粘合剂树脂和溶剂，其特征在于，
上述溶剂含有作为溶解性参数的SP值为10以上的第1溶剂、和上述SP值为8以上但不足10的第2溶剂，
相对于上述溶剂的总质量100质量％，含有20～60质量％的上述第2溶剂。
2.如权利要求1所述的生片材用涂料，其中，上述溶剂中的第2溶剂相对于第1溶剂的质量比为0.2～2.0。
3.如权利要求1或2所述的生片材用涂料，其中，进一步含有分散剂，上述分散剂为聚乙二醇系非离子分散剂。
4.如权利要求3所述的生片材用涂料，其中，上述分散剂的SP值为8～9。
5.如权利要求1～4中任一项所述的生片材用涂料，其中，上述第1溶剂为醇类，上述第2溶剂含有酮类、酯类、芳香族类中的至少一种。
6.如权利要求5所述的生片材用涂料，其中，上述第1溶剂为选自甲醇、乙醇、丙醇、丁醇中的至少一种，上述第2溶剂含有选自甲乙酮、甲基异丁基酮、乙酸乙酯、乙酸丁酯、甲苯、二甲苯中的至少一种。
7.如权利要求1～6中任一项所述的生片材用涂料，其特征在于，上述缩丁醛树脂为聚缩丁醛树脂，上述聚缩丁醛树脂的聚合度为1000以上1700以下，树脂的缩丁醛化度大于64％小于78％，残留乙酰基量不足6％。
8.如权利要求1～7中任一项所述的生片材用涂料，其中，相对于上述陶瓷粉体100质量份含有5质量份以上6.5质量份以下的上述粘合剂树脂。
9.如权利要求1～8中任一项所述的生片材用涂料，其中，上述陶瓷粉体的粒径为0.01～0.5μm。
10.如权利要求1～9中任一项所述的生片材用涂料，其中，上述生片材用涂料中的不挥发成分为10～48质量％。
11.一种陶瓷生片材的制备方法，其包括：
准备权利要求1～10中任一项所述的生片材用涂料的工序，和
使用上述生片材用涂料成形陶瓷生片材的工序。
12.一种陶瓷电子部件的制备方法，其包括：
准备权利要求1～10中任一项所述的生片材用涂料的工序，
使用上述生片材用涂料成形陶瓷生片材的工序，
使上述生片材干燥的工序，
通过内部电极层层压干燥后的生片材，得到生片的工序，和
烧结上述生片的工序。
13.使用权利要求1～10中任一项所述的生片材用涂料制备的生片材。
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| JP320948/2003 | 2003-09-12 | ||
| JP2003320948A JP3808853B2 (ja) | 2003-09-12 | 2003-09-12 | グリーンシート用塗料、グリーンシート、グリーンシートの製造方法および電子部品の製造方法 |
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| US (1) | US7666268B2 (zh) |
| JP (1) | JP3808853B2 (zh) |
| KR (1) | KR100776477B1 (zh) |
| CN (1) | CN100408513C (zh) |
| TW (1) | TWI241603B (zh) |
| WO (1) | WO2005026078A1 (zh) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105518805A (zh) * | 2013-09-17 | 2016-04-20 | 株式会社村田制作所 | 导电性糊剂以及陶瓷电子部件 |
| CN112277493A (zh) * | 2020-10-28 | 2021-01-29 | 中科传感技术(青岛)研究院 | 一种多层压电陶瓷片底面电极转印方法 |
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| JP5040031B2 (ja) * | 2007-06-13 | 2012-10-03 | 株式会社トッパンＴｄｋレーベル | 焼成用転写フィルム |
| KR20130049362A (ko) * | 2011-11-04 | 2013-05-14 | 삼성전기주식회사 | 적층 세라믹 커패시터 제조 방법 |
| JP2018187894A (ja) * | 2017-05-11 | 2018-11-29 | 株式会社リコー | 立体造形物の製造方法 |
| KR102094454B1 (ko) * | 2017-09-20 | 2020-04-23 | 주식회사 엘지화학 | 질화규소 소결체 제조를 위한 테이프 캐스팅용 슬러리 조성물 |
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| GB1341513A (zh) * | 1971-06-30 | 1973-12-25 | ||
| JPS4990792A (zh) * | 1972-12-30 | 1974-08-29 | ||
| US3953562A (en) * | 1974-07-15 | 1976-04-27 | International Business Machines Corporation | Process for the elimination of dimensional changes in ceramic green sheets |
| JP2506905B2 (ja) * | 1988-03-07 | 1996-06-12 | 松下電器産業株式会社 | 積層磁器コンデンサ用グリ―ンシ―ト |
| JP2866137B2 (ja) | 1990-02-23 | 1999-03-08 | 株式会社日本触媒 | セラミックグリーンシートの製造方法 |
| JPH0672760A (ja) * | 1992-08-26 | 1994-03-15 | Nippondenso Co Ltd | セラミックスグリーンシートの製造方法 |
| JP2943129B2 (ja) * | 1992-12-29 | 1999-08-30 | インターナショナル・ビジネス・マシーンズ・コーポレーション | セラミック組成物、セラミック・グリーン・シートおよび製造方法 |
| JPH06206756A (ja) | 1993-01-11 | 1994-07-26 | Matsushita Electric Ind Co Ltd | セラミックグリーンシート用スラリー及び積層セラミックコンデンサ |
| US5660781A (en) * | 1994-06-28 | 1997-08-26 | Sumitomo Metal Industries, Ltd. | Process for preparing glass ceramic green sheets |
| JP3429126B2 (ja) * | 1996-01-09 | 2003-07-22 | 日本碍子株式会社 | 微細貫通孔を有するセラミック部材の製造方法 |
| JPH11144992A (ja) * | 1997-11-12 | 1999-05-28 | Taiyo Yuden Co Ltd | セラミックシートの製造方法 |
| JP2000335971A (ja) | 1999-05-28 | 2000-12-05 | Nippon Tungsten Co Ltd | 水系の溶剤から成る電子部品用セラミックススラリー組成物及びグリーンシートの製造方法 |
| JP3812243B2 (ja) | 1999-10-18 | 2006-08-23 | 株式会社村田製作所 | キャリアフィルム付きセラミックグリーンシートの製造方法 |
| JP2001114569A (ja) * | 1999-10-20 | 2001-04-24 | Murata Mfg Co Ltd | セラミックスラリー組成物、セラミックグリーンシート及び積層セラミック電子部品の製造方法 |
| JP2001167971A (ja) * | 1999-12-13 | 2001-06-22 | Murata Mfg Co Ltd | 積層型セラミック電子部品およびその製造方法 |
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| JP2003176179A (ja) * | 2001-12-11 | 2003-06-24 | Kyocera Corp | セラミックグリーンシートの製法および積層型電子部品の製法 |
| JP2004186396A (ja) * | 2002-12-03 | 2004-07-02 | Murata Mfg Co Ltd | 積層セラミック電子部品の製造方法 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105518805A (zh) * | 2013-09-17 | 2016-04-20 | 株式会社村田制作所 | 导电性糊剂以及陶瓷电子部件 |
| CN105518805B (zh) * | 2013-09-17 | 2018-01-12 | 株式会社村田制作所 | 导电性糊剂以及陶瓷电子部件 |
| CN112277493A (zh) * | 2020-10-28 | 2021-01-29 | 中科传感技术(青岛)研究院 | 一种多层压电陶瓷片底面电极转印方法 |
Also Published As
| Publication number | Publication date |
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| KR20060087563A (ko) | 2006-08-02 |
| JP3808853B2 (ja) | 2006-08-16 |
| KR100776477B1 (ko) | 2007-11-28 |
| CN100408513C (zh) | 2008-08-06 |
| US20070039680A1 (en) | 2007-02-22 |
| JP2005089199A (ja) | 2005-04-07 |
| TWI241603B (en) | 2005-10-11 |
| WO2005026078A1 (ja) | 2005-03-24 |
| TW200514109A (en) | 2005-04-16 |
| US7666268B2 (en) | 2010-02-23 |
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