CN101448759A - 陶瓷材料、烧结陶瓷和由其制成的元件、制造方法和陶瓷的应用 - Google Patents

陶瓷材料、烧结陶瓷和由其制成的元件、制造方法和陶瓷的应用 Download PDF

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CN101448759A
CN101448759A CNA200780018655XA CN200780018655A CN101448759A CN 101448759 A CN101448759 A CN 101448759A CN A200780018655X A CNA200780018655X A CN A200780018655XA CN 200780018655 A CN200780018655 A CN 200780018655A CN 101448759 A CN101448759 A CN 101448759A
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pottery
phase
pure phase
ceramic
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CN101448759B (zh
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P·杜德塞克
C·霍夫曼恩
M·瓦兰特
D·苏沃罗夫
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SnapTrack Inc
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Epcos AG
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Abstract

本发明涉及陶瓷材料、烧结陶瓷和由其制成的元件、制造方法和陶瓷的应用。提供了一种陶瓷混合系，由纯组分A和B的两相混合物组成，其中A相基于Bi3NbO7的立方体至四面体变体，而B相基于Bi2(Zn2/3Nb4/3)O7的单斜晶的烧绿石变体。由此制成的陶瓷物体的电性能使该材料适用于具有多层结构的元件，这种元件中集成有电容和电感器，并且可以用在数据处理或者信号处理中。

Description

陶瓷材料、烧结陶瓷和由其制成的元件、制造方法和陶瓷的应用
技术领域
LTCC(低温共烧陶瓷)工艺可以用来实现具有多个金属化平面的陶瓷多层元件，其中可以集成有多个无源器件如印制导线、电阻、电容和电感器。因此在LTCC陶瓷基底里可以实现电路和包括有这些电路的元件。
背景技术
LTCC工艺可以使电容的集成越强，那么所应用的陶瓷材料的介电常数越高。另一方面，介电常数太高对于电感器的集成是不利的，因此必须对于有关陶瓷的介电常数的选择进行优化。其它对于陶瓷材料的要求在于足够低的烧结温度，以便可以应用成本低的电极材料，例如由银制成。除此之外陶瓷材料应该具有其介电性能和其余性能的低的温度历程，以便可以在宽的温度间隔中使用按LTCC工艺制成的元件，而不会使材能有不许可的变化。
以前还没有这样的陶瓷材料，它在足够低的烧结温度时介电常数大于20，或者其介电常数具有必要的温度稳定性，而且它可以采用LTCC工艺来进行加工。
发明内容
本发明的任务因而是提出一种陶瓷材料，由该材料可以实现所述类型的元件，而并无所提到的缺点。
该任务通过一种具有权利要求1的特征的陶瓷材料来解决。本发明的有利构造方案，一种由该材料制成的烧结陶瓷、一种由该陶瓷制成的元件，以及制造方法和优选的应用都可以见其它的权利要求。
提供了一种陶瓷材料，它由两个纯相A相和B相的混合物组成。相混合物的组成为xA+(1-x)B，其中0<x<1。A相是Bi3NbO7的一种立方体至四面体变体。B相基于Bi2(Zn2/3Nb4/3)O7系的一种单斜晶的烧绿石变体。在混合物中，这两个A相和B相分别形成纯相区域。
根据确定了纯相的晶体结构的所述基本组成成分，两个相中的每个相因此是可以变化的，因此在整个材料中的元素Bi、Zn和Nb分别直至30摩尔百分比的份额被其它的金属代替。除此之外铌可以完全用钽代替。其它以替代方式按份额存在的金属优选这样来选择，即它们在类似的原子直径时具有相同的或者类似的原子价，从而它们可以没有问题地在其晶格位置上代替原始元素，或者相应的结晶相不会有过大的晶格变形。
直至30摩尔百分比份额的铋尤其可以通过一种或多种元素来代替，上述元素由以下选择：Ca、Sr、Ba、Pb、Cd、Y、La和原子序数从58至71的稀土元素。相应的元素代替不会在两个结晶学的A相和B相里引起晶体变体的改变。
在B相里，直至30摩尔百分比的锌可以通过一种或多种元素来代替，所述元素从以下选择：Mg、Ca、Co、Mn、Ni、Fe、Cr和Cu。这里通过相应的替代也并不影响晶体变体。
元素铌可以在两个纯相的任意一个相中直至30摩尔百分比的份额通过一种或多种元素来代替，所述元素可由以下元素中选择：Sn、Ti、Hf、Sb、Ta、V、W和Mo。这些替代也并不引起晶体变体的改变。此外Nb完全可以替换Sb，纯相或者混合相中的相不会因此而改变。
所提供的陶瓷材料的有利的组成成分可以在三种元素Zn-Nb-Bi的相图中通过四个构成了四角形的点A、B、C、D来确定。位于四角形之内的组成成分按照本发明是很好适合的，并且尤其具有适合的低的烧结温度，足够高的介电常数和高的介电品质。四个点A至D如下通过它们在陶瓷材料中以摩尔百分比所说明的份额来确定：
A：Zn＝4.0；Nb＝30.0；Bi＝66.0
B：Zn＝7.8；Nb＝25.0；Bi＝67.2
C：Zn＝16.0；Nb＝30.0；Bi＝54.0
D：Zn＝15.0；Nb＝35.0；Bi＝50.0
由所述的材料，在烧结温度低于960℃，有利地局部甚至低于900℃时可以烧结陶瓷物体。可以得到的陶瓷的介电常数在65和95之间。这样的陶瓷同时可以具有大于800的介电品质，分别在测量频率为1千兆赫时测定。
在一种有利的陶瓷中，A相在陶瓷材料中的摩尔份额x在0.1到0.8之间。例如两种相A相和B相的一种1:1的混合物是特别适合的。一种纯相A和B的份额近似相等的陶瓷组成成分的主要优点在于：按这种方式，材料的温度常数和尤其是两个纯相的介电常数的温度系数得以平衡，并因此在陶瓷材料中总体上可以实现最小化。这是由于纯相B具有介电常数的负的温度系数，而纯相B则相反具有正的温度系数。用一种1:1的A相和B相的相混合物在-44°到+155℃之间例如得到介电常数的温度系数(通过由此制成的介电谐振器的谐振频率来确定)只是-5ppm。这种陶瓷的ε为81，介电品质Q为1000(在1千兆赫时测量)，或者乘积Q*f＝1000千兆赫。
按照本发明的陶瓷材料除此之外还有另外的优点：在温度直到超过烧结温度时相比于含银的电极材料来说是惰性的。这就允许采用含银的电极对由陶瓷材料构成的生坯进行压印并一起烧结成制成的元件，而相组成成分不会由于用银替代单个元素或者由于附加地加入银而发生变化。因而陶瓷材料和由此制成的陶瓷相当出众地适用于陶瓷元件，尤其是在应用了成本低的银电极条件下适用于陶瓷的多层元件。
如果A相和B相以规定的初始组成成分存在，那就能可靠地得到所述的良好性能。除了用钽代替铌，这可以直至100％进行替代，而并不使陶瓷的性能因此而重大改变，然而通过所述代替原子来部分地代替单个的或者多个元素使性能发生变化，使得只有达到所述大约为30摩尔百分比的份额的代替，才形成对于所述使用目的来说适用的陶瓷。
例如以下情况可能会造成限制：由于不适合的相混合比例以及铋的高替代，在整个陶瓷里铋的份额降低得太多。在这些情况下可以观察到陶瓷材料相比于含银的电极材料其稳定性变差了，这造成相的变体具有不确定的组成成分，其在一定条件下具有并不适合的性能，另外其难以进行控制。如果铋份额在整个陶瓷材料中达到大于50摩尔百分比的话，那就得到一种可靠的稳定性。但是在个别情况下，可以得到具有较少铋份额的陶瓷组成成分，它们在烧结时相对于含银的材料来说是稳定的。
一种用陶瓷材料或者用由此烧结出的陶瓷所制成的元件可以有利地构造成具有多层结构，其中在单块的陶瓷物体中，多个陶瓷层用位于它们之间的金属化平面替换。陶瓷层在堆叠中一起烧结，其中由结构化的金属化平面形成无源器件或者无源器件的连接，这些金属化器件通过触通通孔相互连接起来。
无源器件的电路布线总的可以形成完整独立的元件，它例如构造成用于移动通信应用的LC滤波器。也可以应用一种由所述的陶瓷材料制成的具有集成在其中的无源器件的多层陶瓷作为电气元件的基底，尤其是作为用于具有各种不同的电气元件的模块的基底。这种基底可以形成必需要的电路布线以及为此所必需的匹配元件，用于那些集成在模块上的单个器件或IC(集成电路)。
为了制成按照本发明的陶瓷材料，从作为已知的纯相A和B出发。A相例如在文章“Solid Solutions Bi2O3-Nb2O5(固溶体Bi2O3-Nb2O5)”(作者为M.Valant和D.Suvrov，发表示J.Am.Cer.Soc.86[6]939-944(2003))里作了说明。B相例如在文章“Structures，phase transformationsand dielectric properties of pyrochlores containing Bi(含有铋的烧绿石的结构、相变和介电特性)”(作者X.VWang，发表于J.Am.Cer.Soc.80[10]2745-2748(1997))中作了说明。这些纯相相互分开地被制成，其中有利地使用所谓混合氧化物方法。为此将氧化物形式的单个元素以所希望的摩尔比例相互混合，磨成粉未混合物并均质化，接着经历适合的温度程序，这种程序导致A相或者B的所希望的晶体变体。纯相有利地用两阶段煅烧法和烧结法制成，其中第一阶段在低温下进行，以避免挥发相从铋氧化物里太强烈地挥发，并因此避免铋材料的减少。
在制造纯相B时有利地在大约800℃时的较长时间地保持，以便可以实现至少局部地从立方体相至优选四面体相的相转变。然而一种按照本发明的陶瓷材料也可以具有这样的B相，它并不完全转变成四面体相，但具有所希望的性能。
在制成纯相之后将它们分别磨到小于2μm的颗粒大小。具有纯相的粉末以给定的用于两相混合物的混合比例进行混合、均质化并由此制成生膜。但是磨成所述颗粒大小也可以在纯相混合之后进行。
在生膜里接着例如通过冲压产生触通通孔并填装上导电材料，例如含有金属颗粒的膏糊。接着对含有金属的能够烧结的膏糊形式的金属化结构进行压印。
接着使多个这种薄膜如此堆叠起来，使得通过触通通孔实现了金属化结构的适合的电路布线，这些金属化结构与位于它们之间的陶瓷共同作用就可以实现所希望的元件功能。
接着通过层压将堆叠的薄膜固定住。在该工艺过程之后，原始的大面积地制成的包含有多个单个元件或者用于元件的单个基底的多层陶瓷通过分割过程，例如通过切割而分离。接着将层压过的生膜烧结。
业已表明，一次制成的纯相即使在两相混合物的均质混合中，直到超过烧结温度在热力学方面也是稳定的，因此在混合物中也不用担心发生相转变。在烧结过程中只是使生膜压缩，其中可以使整个烧结过程快速实施。使之快速地加热到例如900℃的烧结温度，在那里短暂保持并接着快速冷却。
附图说明
以下根据实施例和附属的图对本发明详细加以说明。
图1表示Nb、Bi和Zn系的三相图的局部，在此图中标有有利的组成成分；
图2说明了制造元件的工序流程图；
图3表示了一种按本发明制成的元件的示意截面图；
图4借助图片表示一种具有按本发明的所述组成成分的陶瓷的陶瓷结构。
具体实施方式
图1表示了ZnO-BiO1，5-NbO2，5三相图的局部。在该相图中通过四个点A至D形成四角形，在该四角形中，由这些点围成的面中的每个点都代表了一种具有有利性能的按照本发明的陶瓷的一种组成成分。以摩尔百分比表示的不同点A、B、C和D的坐标如下：
A：Zn＝4.0；NbO2，5＝30.0；BiO1，5＝66.0
B：Zn＝7.8；Nb＝25.0；Bi＝67.2
C：Zn＝16.0；Nb＝30.0；Bi＝54.0
D：Zn＝15.0；Nb＝35.0；Bi＝50.0
此外还在相图中标出了三个用X表示的并且位于一条线上的组成成分。两个外面的点由两个纯相A或B构成。在直线中间的点相当于两个纯相的一种1:1组成成分。这种实施方式具有近似最佳的性能，这使烧结陶瓷很好地适合应用在这样的电气元件中，在这些电气元件中实现了一种电容和/或一种电感器并且适合于使用在高频技术中，尤其适合用于应用在无线通信系统中的元件。这种所列出的1:1组成成分如前所述，其介电常数ε为81，品质因子Q为1000(在1千兆赫时测定)、谐振频率的温度系数，在由这种陶瓷制成的介电谐振器上测定为-5ppm且品质与频率的乘积为1000千兆赫。
高的介电常数是特别有利的，它可以使相应的元件实现微型化，还特别有利的是小的温度系数，该系数以按照本发明的方式由两个纯相A和B的相反的温度系数得出，上述纯相在按照本发明的陶瓷混合物中是平衡的。混合相的烧结温度大大低于纯相B的烧结温度，后者高于950°。如所述的1:1的混合相那样，组成接近为1:1组成成分的混合相具有类似有利的性能。一般来讲，对于接近于纯相A和B的组成成分来说，对于所述的或者所希望使用目的的性能而言是相对最不利的。然而对于所有按照本发明的混合相来说，它们相比于纯相而言具有改善的性能，尤其是改善的温度系数。例如从1:9至9:1的混合比例A:B具有良好适合的性能。一般在纯相B附近比在纯相A附近具有更加有利的性能。
图2表示了一种多层电气元件的制造方法流程图，其具有多层按照本发明的组成成分的陶瓷。在第一步里相互分开地制造纯相A和B，优选在混合氧化物方法之后。将金属氧化物以电子等级质量混合成纯相所必需的比例，进行磨碎并均质化，并接着煅烧和烧结。煅烧优选分两阶段进行，其中第一级在相对低的温度时进行，以避免挥发性的铋相过强地挥发掉。对于组分A来说，在800℃时保持较长的时间，此时发生至少局部的从初始产生的立方体相至四面体相的转变。尤其是四面体相按照本发明是适合的，但它还包含有立方体相的成分，但这并不对按照本发明的陶瓷组成成分的性能在它们的电气特性方面产生不利的影响。纯相B作为单斜晶的烧绿石产生。
在下步骤中将纯相A和B以一种所希望的比例结合、混合和磨细，直至颗粒直径为2μm和更小。通过两个纯相的共同研磨也产生了具有纯相区域的磨细的颗粒的均质混合。
在下一步骤中，由均质化混合的相制成生膜。为此通过一种溶剂，必要时该溶剂可以包含有胶粘的粘合剂成分，将磨细的粉末结合起来并由此制造生膜，例如通过薄膜拉伸或者薄膜注塑。在下一步骤中，在干燥并将溶剂与生膜分离开之后，产生出对于所需要的元件来说必需的触通通孔，例如通过冲压。这种触通通孔接着装满一种能导电的、含有金属颗粒的物质，这例如可以用刮板来进行。最后在生膜上压印上金属化结构，例如通过丝网印制法。产生于生膜上的金属化结构相当于以后的多层陶瓷里的金属化平面。
下一步将压印的生膜以对于元件来说正确的次序上下堆叠起来并压成紧密的物体。该物体已经具有一定的机械强度并可以有利地在该阶段通过切割或者冲压来分离。这是必需的，这是因为生膜通常用大的底面制成，在该底面上可以并排地制成用于多个相同的或者不同元件的金属化结构。通过分割将这些元件分离。
下一步将分离的薄膜堆叠进行烧结。得到一种单块的陶瓷多层元件，在该多层中，通过在以触通通孔相互连接的不同金属化平面中的金属化结构的共同作用，实现了不同的有源元件的功能，例如电容和电感器。在单块的陶瓷元件上，可以在最后步骤中涂覆外部电极，只要这些外部电极在烧结之前没有集成地在生膜上涂覆过。
图4在按照本发明的实心陶瓷物体的抛光截面中示出了它的陶瓷结构。图片表明，混合相由连续的相构成，这个相可以主要属于纯相A。其中亮点表示夹杂物，它们可以属于纯相B。黑的点或范围是试样的残留气孔或者污物。由图也可以见到，在烧结时发生了晶粒生长。可以见到晶粒直径通常直至5μm，部分直径直至大约10μm。
图3表示了一种可能的元件，如同用按照本发明的由两个相组成的混合陶瓷可以得到或者实现的那样。这里所示的元件例如具有六个上下相互堆叠的和烧结起来的陶瓷层K1至K6。在每两个陶瓷层K之间有金属化平面，在该平面里构成有金属化结构M。在不同金属化平面的金属化结构M之间必需的电连接通过所述的触通通孔DK来实现。
在图3中简略地表示了两个元件，也就是电容C，它由两个在相邻的金属化平面中布置的金属表面构成。在其旁边表示出有电感器L，它例如作为螺旋线状的构造由多个通过触通通孔相互连接起来的半环组成。在陶瓷物体的底面上设有外部接头AK、AK’，用这些外部接头，元件可以与外面的电路环境接通。这样的元件例如可以构造成LC滤波器，在该滤波器中，L部分和C部分的适合的电路布线实现一种带通，如同在移动通信的终端设备中可以应用的那样。
也可以将按照本发明的多层陶瓷作为基底应用于其它元件，为此多层陶瓷除了在底面上的外部接头之外，附加地还在顶面上具有连接表面(图中未示出)，在这些连接表面上是分立的或者集成的元件，或者任意的元件芯片，例如以声表面波进行工作的元件的设有金属化结构的压电晶体。
通过本发明的陶瓷所实现的陶瓷元件的金属化结构可以由银或者任意其它的耐烧结温度的金属构成。触通通孔同样也可以填有含银材料或者银钯合金。陶瓷可以构造成具有多层结构的致密物体。也可以相应地结构化的生膜连接成多层堆叠并烧结，在该堆叠里实现三维的结构。因此例如可以在多层堆叠里实现空腔，它可以是敞开的或者是封闭的。在敞开的空腔里例如可以布置分立的元件，并与金属化结构连接。这可以实现一种特别紧凑的元件。
本发明并不局限于个别所示的实施例。在本发明范围里有其它的组成成分，此时纯相的金属成分在所述范围里直至最大30摩尔百分比被通过所述代替原子来替换。对于替换和由此达到的陶瓷性能来说决定性的是，要保持纯相的各自晶体结构。因此一般可以没有问题地使原子价和原子直径相似的金属进行替换。按照本发明的两种纯相A和B的混合物也有这样的组成成分，它们只含有少量份额的两种相中的一个，并因此主要由另一个纯相组成。每个混合相相比于纯相具有一种就所希望的性能谱来说更好的特性。
由这种陶瓷制成的元件也并不限于所述的实施方式。原则上可以由这种陶瓷制造多个不同的电陶瓷元件，然而陶瓷特别适用于这样的元件，即在这些元件中集成有各种不同的无源器件。这样的元件可以被优选地使用在元件并不是用最大功率加载的地方，如尤其是在信号或数据处理元件中时那样。

Claims (21)

1.陶瓷材料，由两相混合物xA+(1-x)B组成，
-其中0<x<1，
-其中A相基于Bi3NbO7的立方体至四面体变体，
-其中B相基于Bi2(Zn2/3Nb4/3)O7的单斜晶的烧绿石变体，
-其中两个相能够如此变化，使得Bi、Zn和Nb在整个材料中分别直至30摩尔百分比的份额被其它金属代替，而Nb能够直至100％被Ta代替。
2.按权利要求1所述的材料，在此材料中，Bi直至30摩尔百分比的份额由下述元素中的一种或多种来代替，所述元素由以下选出：Ca、Sr、Ba、Pb、Cd、Y、La和原子序数从58至71的稀土元素。
3.按权利要求1或2所述的材料，在此材料中，Zn直至30摩尔百分比的份额由下述元素中的一种或多种代替，所述元素由以下选出：Mg、Ca、Co、Mn、Ni、Fe、Cr和Cu。
4.按权利要求1至3中之一所述的材料，在此材料中，Nb直至30摩尔百分比的份额由下述元素中的一种或多种代替，所述元素由以下选出：Sn、Ti、Hf、Sb、Ta、V、W和Mo。
5.按权利要求1至4中之一所述的材料，其在元素Zn-Nb-Bi的相图中通过四个点A、B、C和D来确定，四个点为：
A：Zn＝4.0；Nb＝30.0；Bi＝66.0
B：Zn＝7.8；Nb＝25.0；Bi＝67.2
C：Zn＝16.0；Nb＝30.0；Bi＝54.0
D：Zn＝15.0；Nb＝35.0；Bi＝50.0。
6.由按权利要求1至5中之一所述材料制成的烧结陶瓷，烧结温度低于960℃。
7.按权利要求6所述的陶瓷，介电常数为65-95。
8.按权利要求6或7所述的陶瓷，在测量频率为1GHz时，介电品质大于800。
9.按权利要求6至8中之一所述的陶瓷，在此陶瓷中，A相在陶瓷材料中的相对摩尔份额x为0.10至0.80。
10.按权利要求6至8中之一所述的陶瓷，在此陶瓷中，所述相在混合物中作为主要成分的纯相存在。
11.按权利要求6-10中之一所述的陶瓷，在此陶瓷中，纯相A和B的区域直径小于等于10μm。
12.电气元件，包括有按权利要求6-11中之一所述的陶瓷。
13.按权利要求12所述的元件，包括无源器件的电路布线，该电路布线构造在多层结构中，在该多层结构中设有由所述陶瓷制成的多个陶瓷层，这些陶瓷层交替地具有结构化的金属化平面，并且所述多个陶瓷层烧结成单块的堆叠，在此堆叠中，结构化的金属化平面通过触通通孔相互连接，并因此形成无源器件的电路布线。
14.按权利要求13所述的元件，构造成LC滤波器。
15.按权利要求12或13所述的元件，构造成用于电气元件的基底。
16.按权利要求1至5中之一所述陶瓷材料的制造方法，在此方法中，首先相互分开地制成纯相A和B；在此方法中，将纯相研磨成粉末；在该方法中，将具有两个纯相的粉末以规定的比例进行混合。
17.按权利要求16所述的方法，在此方法中，将混合物加工成生坯并进行烧结。
18.按权利要求16所述的方法，在此方法中，纯相分别按照混合氧化物方法制成。
19.按权利要求16至18中之一所述的方法，在此方法中，在小于960℃的温度时进行烧结。
20.按权利要求16至19中之一所述的方法，
-在此方法中，制成薄膜作为生坯；
-在此方法中，在薄膜中冲压触通通孔并填上能导电的材料；
-在此方法中，用由电极材料制成的金属化结构对薄膜进行压印；
-在该方法中，将多个不同的薄膜上下堆叠起来、进行层压和烧结。
21.按照权利要求12至15中之一所述元件的应用，用于采用低温共烧陶瓷工艺制造移动通信应用领域中的LC滤波器，应用于频率范围1-5GHz。
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CN104098327A (zh) * 2013-04-04 2014-10-15 Tdk株式会社 电介质陶瓷组合物、电介质陶瓷、电子部件以及通信设备
CN104098327B (zh) * 2013-04-04 2016-03-23 Tdk株式会社 电介质陶瓷组合物、电介质陶瓷、电子部件以及通信设备
CN110171965A (zh) * 2019-04-26 2019-08-27 武汉理工大学 一种npo电容器介质材料及其制备方法
CN110372377A (zh) * 2019-07-24 2019-10-25 天津大学 一种巨介电常数电介质材料的制备方法
CN111540604A (zh) * 2020-05-07 2020-08-14 无锡太湖学院 一种多层片状陶瓷电子元器件的制备方法
CN111540604B (zh) * 2020-05-07 2022-05-31 无锡太湖学院 一种多层片状陶瓷电子元器件的制备方法
CN114956816A (zh) * 2022-06-07 2022-08-30 清华大学 一种高性能烧绿石储能陶瓷材料及其制备方法与应用

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CN101448759B (zh) 2013-06-19
KR20090015130A (ko) 2009-02-11
JP2009537444A (ja) 2009-10-29
TWI400214B (zh) 2013-07-01
WO2007134569A2 (de) 2007-11-29
WO2007134569A3 (de) 2008-03-06
US20090155624A1 (en) 2009-06-18
KR101339090B1 (ko) 2013-12-09
US7816293B2 (en) 2010-10-19

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