CN1266079C - 陶瓷材料及其制备方法 - Google Patents

陶瓷材料及其制备方法 Download PDF

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CN1266079C
CN1266079C CNB2004100330741A CN200410033074A CN1266079C CN 1266079 C CN1266079 C CN 1266079C CN B2004100330741 A CNB2004100330741 A CN B2004100330741A CN 200410033074 A CN200410033074 A CN 200410033074A CN 1266079 C CN1266079 C CN 1266079C
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木岛健
名取荣治
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Seiko Epson Corp
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Abstract

一种涂覆用陶瓷材料的制备方法，其中，包括在铂族元素催化剂的存在下，搅拌含有复合氧化物的原材料的工序。原材料是含有选自复合氧化物的水解物和缩聚物中至少一种的溶胶·凝胶原料。

Description

陶瓷材料及其制备方法
技术领域
本发明涉及涂覆用陶瓷材料及其制备方法。
背景技术
目前，作为适用于半导体装置(例如，强电介质存储器(FeRAM))的强电介质膜，提出了具有钙钛矿结构的强电介质膜(例如，PbZrTiO系)或具有层状钙钛矿结构的强电介质膜(例如BiLaTiO系、BiTiO系、SrBiTaO系)。
作为这些强电介质膜的形成方法，已知正在使用的有溶胶·凝胶材料或MOD材料的涂覆法。该涂覆法与溅射法相比具有比较容易控制膜的组成，不产生颗粒等特征。
发明内容
本发明的目的是提供一种可以获得膜特性优良的陶瓷膜的涂覆用陶瓷材料的制备方法，以及该陶瓷材料。
本发明的涂覆用陶瓷材料的制备方法包括在铂族元素催化剂的存在下，搅拌含有复合氧化物的原材料的工序。
根据本发明，在铂族元素催化剂的存在下，通过搅拌复合氧化物，可以制得具有优异膜特性的陶瓷膜的陶瓷材料。
在本发明的制备方法中，前述原材料可以是含有前述复合氧化物的水解产物和聚合物中至少一种的溶胶·凝胶原料。或者根据需要，前述原材料还可以是含有MOD原料的溶胶·凝胶原料。
在本发明的制备方法中，前述原材料除了含有前述复合氧化物以外，其中还可以加入对该复合氧化物有催化作用的常电介质材料。这时，前述常电介质材料可以由构成元素中含有Si或Ge的氧化物、或构成元素含有Si和Ge的氧化物组成。
本发明的涂覆用陶瓷材料是通过本发明的涂覆用陶瓷材料的制备方法制成的。
附图说明
图1是模式表示的本发明的制备方法的图。
图2A、B是表示实施例和比较例中的样品的PZT膜的磁滞特性图。
图3A～图3D是表示实施例中样品的PZT膜的磁滞特性的图。
具体实施方式
下面就本发明的实施方式的一个例子进行说明。
在本实施方式中，涂覆用陶瓷材料的制备方法包括在铂族元素催化剂的存在下，搅拌含有复合氧化物的原材料的工序。也就是说，如图1所示，在本实施方式中，在容器1中加入铂族元素催化剂2和含有复合氧化物的原材料3。然后，由搅拌机4搅拌原料3得到陶瓷材料。通过搅拌原材料3可以使得铂族元素催化剂2和原材料3高效率地非常均匀地接触。这样配制出的陶瓷材料如后面的实施例中所记载，可以得到膜特性优异的陶瓷膜，而且其性质趋于稳定，不会随着时间而改变。
关于由于铂族元素催化剂的存在而能得到优异的陶瓷材料的原因，认为可能是由于铂族元素的催化作用，促进了溶胶·凝胶原料的醇交换反应。
作为铂族元素催化剂可以列举的有，铂、钌、铑、钯、锇、铱，作为催化剂的形态可以是板状、筛状、颗粒状等，但并不局限于此，可以使用各种型态。考虑到增大催化剂和原材料的接触面积、优选的催化剂是筛状、颗粒状的形态。催化剂在原料搅拌结束时除去。
在本实施方式中，原材料可以是选自含有复合氧化物的水解产物和缩聚物中至少一种的溶胶·凝胶原料。或者根据需要，前述原材料可以是含有MOD原料的溶胶·凝胶原料。
溶胶·凝胶原料具体地可以根据如下方法调节。首先，混和碳原子数为4以下(其中“以下”是指“小于和等于”，下述相同)的金属醇盐后，进行水解和缩聚。通过该水解和缩聚，可以产生牢固的M-O-M-O…键。此时得到的M-O-M键具有与陶瓷的晶体结构(钙钛矿结构)相似的结构。这里，M是金属元素(例如，Bi、Ti、La、Pb等)，O表示氧。接着，在水解和缩聚而得到的产物中加入溶剂，得到原料。这样可以调配溶胶·凝胶原料。
作为MOD原料可以列举的有，例如陶瓷膜的构成元素之间相互直接或间接地连续连接的多核金属配位化合物原料。MOD原料具体可以列举羧酸的金属盐。作为羧酸可以列举的有醋酸、2-乙基己酸等。作为金属可以列举的有，例如Bi、Ti、La、Pb等。与溶胶·凝胶原料相同，MOD原料也具有M-O键。但是，其M-O键不是像通过缩聚得到的溶胶·凝胶原料那样连续地结合而成的，另外，键的结构也和与接近线性结构的钙钛矿结构相差甚远。
另外，原材料可以通过调节溶胶·凝胶原料或MOD原料等复合氧化物使其达到化学计量的组成，并且在这些混合物中，对于含有复合氧化物的金属材料(例如，Pi、Bi等)，可以以相对于前述化学计量组成过量的量存在。
根据本实施方式，原材料中除了前述复合氧化物以外，还可以含有对复合氧化物有催化作用的常电介质材料。除了在原材料中加入构成强电介质的复合氧化物之外，通过混合常电介质材料，在复合氧化物的结晶过程中，复合氧化物部分构成元素可以与常电介质材料的构成元素置换而降低结晶化温度。
这里，常电介质材料可以由在其构成元素中含有Si或Ge的氧化物，或在其构成元素中含有Si和Ge的氧化物构成。
作为这样的常电介质材料可以采用的有，例如在构成元素中含有Si或Ge的氧化物，或在构成元素中含有Si和Ge的氧化物。这样的氧化物是以ABOx或BOx表示的常电介质材料，可以采用A位置由Pb、Bi、Hf、Zr、V、W中的任一种单一元素或复合元素形成，B位置由Si、Ge中的任一种单一元素或复合元素形成的材料。具体可以列举的有，PbSiO系(Pb5Si3Ox、Pb2Si1Ox)、PbGeO系(Pb5Ge3Ox、Pb2Ge1Ox)、BiSiO系(Bi4Si3Ox、Bi2Si1Ox)、BiGeO系(Bi4Ge3Ox、Bi2Ge1Ox)、ZrGeOx、HfGeOx、VGeOx、WGeOX、VSiOx、WSiOx等。另外，在A位置中使用Zr、Hf、V、W时，具有抑制强电介质的氧缺损的效果。
在本实施方式中，涂覆用陶瓷材料是在铂族元素催化剂的存在下，搅拌原材料，并除去铂族元素催化剂而制备得到的。同时，通过公知的涂覆方法，例如旋转涂覆法、浸渍法将得到的陶瓷材料涂覆在基体上。
本实施方式的陶瓷材料可以通过公知的方法热处理而得到陶瓷膜，例如强电介质膜。比如陶瓷膜可以通过如下方法得到。首先，通过将本实施方式的陶瓷材料旋转涂覆在基体上形成涂覆膜。接着，根据需要，干燥和暂时焙烧涂覆膜。接着，通过热处理涂覆膜，使薄膜结晶而形成陶瓷膜。
接下来，参照附图就本实施方式的涂覆方法的更加详细的实施例进行说明
(实施例)
首先，在放入板状的铂的容器中，对调整至化学计量组成的、用于形成PbZr0.2Ti0.8O3膜的溶胶·凝胶溶液(浓度：l0％重量)进行搅拌，然后除去铂，得到实施例的陶瓷材料样品1。与此相对的，在不加入铂的情况下，以和样品l同样的方法调制陶瓷材料。将该陶瓷材料作为比较样品1。而且，在该实施例中，原材料的Pb过量20mol％。接着，用样品1和比较样品1的陶瓷材料制备成涂覆膜。通过旋转涂覆法将样品1与比较样品1的溶胶·凝胶溶液涂覆在铂电极上形成涂覆膜。这时，旋转涂覆在3000rpm下进行30秒。接着使用加热板，在150℃下加热涂覆膜2分钟，再在300℃下加热5分钟进行临时焙烧。通过反复进行3次上述的涂覆工序和临时焙烧工序，形成膜厚150nm的涂覆层。
接着，用加压热处理装置，进行涂覆膜的结晶化。进行结晶化的条件为压力9.9大气压、热处理的温度为650℃、处理时间为10分钟。
接着，在涂覆膜上形成直径100um、厚100nm的铂电极，得到电容器。使用该电容器来测定强电介质的特性(磁滞特性)。其结果图2A、B所示。图2A表示本实施例样品1的磁滞特性，图2B表示比较样品1的磁滞特性。从该结果来看，在低电压下本实施例的样品1相对于比较样品1具有饱和矩形性优良的磁滞特性。
接着，为了观察样品1的陶瓷材料随时间的变化，进行以下的测定。即用同样的方法，用刚制备好的陶瓷材料与放置一段时间后的陶瓷材料以上述方法形成电容器样品。然后测定各个样品的磁滞特性。得到如图3A～D所示的结果。图3A、图3B、图3C、图3D分别是使用了刚制备的、制备后2周的、制备后4周的、制备后6周的陶瓷材料的样品的磁滞特性。从这些结果来看，使用本实施例的陶瓷材料的电容器，都具有矩形性优良的磁滞特性，并且，经证实，这些磁滞特性几乎不随制备后陶瓷材料所经过的时间而变化。
综上所述，根据本发明的实施例，在铂族元素催化剂的存在下制备陶瓷材料，可以形成具有良好的强电介质特性的陶瓷材料膜，并且可以得到不随时间变化的陶瓷材料。

Claims (5)

1、一种涂覆用陶瓷材料的制备方法，其中，包括在铂族元素催化剂的存在下，搅拌含有复合氧化物的原材料的工序。
2、根据权利要求1所述的涂覆用陶瓷材料的制备方法，其中，所述原材料是含有选自前述复合氧化物的水解物和缩聚物中至少一种的溶胶·凝胶原料。
3、根据权利要求1或2所述的涂覆用陶瓷材料的制备方法，其中，所述原材料除了含有前述复合氧化物的材料以外，还含有对复合氧化物有催化作用的氧化物材料。
4、根据权利要求3所述的涂覆用陶瓷材料的制备方法，其中，所述有催化作用的氧化物材料是由含有Si或Ge的氧化物材料、或含有Si和Ge的氧化物材料构成。
5、一种涂覆用陶瓷材料，使用权利要求1～4中任一项所述的涂覆用陶瓷材料的制备方法而形成。
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