CN100522881C - 电介质陶瓷组合物及使用其的层压型陶瓷零件 - Google Patents

电介质陶瓷组合物及使用其的层压型陶瓷零件 Download PDF

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CN100522881C
CN100522881C CN200410104734.0A CN200410104734A CN100522881C CN 100522881 C CN100522881 C CN 100522881C CN 200410104734 A CN200410104734 A CN 200410104734A CN 100522881 C CN100522881 C CN 100522881C
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glass
weight
dielectric
amorphous glass
composition
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CN1623958A (zh
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梅本卓史
野野上宽
田沼俊雄
胁坂健一郎
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Sanyo Electric Co Ltd
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Sanyo Electric Co Ltd
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    • B32—LAYERED PRODUCTS
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    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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Abstract

一种含有结晶玻璃、无定形玻璃和陶瓷填充材料的电介质陶瓷组合物，其特征在于，结晶玻璃的软化点比无定形玻璃的软化点高，并且为900℃或其以下，含有27重量%或其以上的结晶玻璃，不足20重量%的无定形玻璃，结晶玻璃和无定形玻璃合计为60重量%或其以下，并且含有40重量%或其以上的陶瓷填充材料。

Description

电介质陶瓷组合物及使用其的层压型陶瓷零件
发明领域
本发明涉及用于层压型陶瓷零件等的电介质陶瓷组合物及其使用其的层压型陶瓷零件。
背景技术
近年来，伴随着电子零件的小型化，薄型化，对层压型陶瓷零件的需求急剧增加。作为层压型陶瓷零件的代表例，使用能同Ag等导电材料同时煅烧的低温煅烧材料(LTCC)，在各层中构成电感器和电容器的电路。作为用于层压型陶瓷零件的低温煅烧的材料，一般使用混合氧化铝等的陶瓷填充材料和玻璃的电介质陶瓷组合物。
为在900℃左右的温度下提高烧结性，需要混合大于60重量％左右的玻璃，然而，如果玻璃添加量增多，则会产生增加原材料成本增大的问题。如果玻璃添加量减少，则不能获得足够的烧结性，存在机械强度及介电特性降低的问题。
发明内容
本发明的目的是提供一种机械强度及介电特性优良的，可在900℃左右的低温下煅烧的电介质陶瓷组合物。
本发明是一种含有结晶玻璃，无定形玻璃和陶瓷填充材料的电介质陶瓷组合物，其特征在于，结晶玻璃的软化点比无定形玻璃的软化点高，且在900℃或其以下，所述陶瓷组合物含有27重量％或其以上的结晶玻璃，不足20重量％的无定形玻璃，结晶玻璃和无定形玻璃合计为60重量％或其以下，含有40重量％或其以上的陶瓷填充材料。
根据本发明，可以得到一种机械强度及电介质特性优良，可以在900℃左右的低温下煅烧的电介质陶瓷组合物。
在本发明中，结晶玻璃的软化点比无定形玻璃的软化点高，且为900℃或其以下。因此，由于在煅烧工序中，结晶玻璃结晶化以前，无定形玻璃软化具有流动性，促进了结晶玻璃粒子与陶瓷填充物粒子的再排序，之后，进行结晶玻璃的软化及结晶化。因此，少量的玻璃成分也能进行900℃左右的低温烧结。因而，在降低成本的同时，可以制成机械强度及介电特性优良的电介质陶瓷基板。
图1是用于说明本发明上述作用效果的示意图。对于本发明的电介质陶瓷组合物，其煅烧工序如图1(a)中所示，无定形玻璃2首先软化，具有流动性。因此，促进了结晶玻璃1粒子与陶瓷填充物3粒子的再排序。在此状态下，如果再接近煅烧温度，如图1(b)中所示，结晶玻璃1发生软化，引起结晶玻璃1的结晶化，结晶相4从结晶玻璃中析出。因此，可以得到机械强度优良并且介电特性好的电介质陶瓷。
在特开2001-84835号公报中，揭示了含有结晶玻璃的组合物，无定形硅酸盐玻璃组合物和陶瓷组合物的绝缘体组合物。但并没有揭示为控制烧结后的热膨胀系数，如何调整结晶玻璃和无定形玻璃的混合比，以及结晶玻璃和无定形玻璃的软化点。另外，记载了如果含有50重量％或其以上的SiO2填充材料，则不能进行低温烧结。
在特开平10-22162号公报中，揭示了一种具有高介电率层和低介电率层的叠层，含有结晶玻璃的复合层压型陶瓷零件，所述结晶玻璃粘合有在低介电率烧结时能流动软化的高介电率层和导体层。其中并没有任何关于结晶玻璃的软化点比无定形玻璃的软化点高的说明，且陶瓷填充物的含量至少为19重量％或其以下。
在本发明中，含有27重量％以上的结晶玻璃，不足20重量％的无定形玻璃。如果结晶玻璃的含量较少，机械强度及介电特性将会降低。结晶玻璃的含量优选为27～58重量％，更优选为30～55重量％。此外，无定形玻璃的含量优选为2～18重量％。
并且，在本发明中，结晶玻璃和无定形玻璃合计为60％重量或其以下，陶瓷填充材料为40重量％或其以上。如果陶瓷填充物的含量少于40重量％，则会降低机械强度及介电特性。
作为在本发明中所使用的陶瓷填充材料，优选使用介电率为5或5以上的材料构成的材料。作为这样的材料，可列举Al2O3(氧化铝)、TiO2(二氧化钛)、Al6Si2O13(莫来石)、ZrO2、CaZrC)3、ZnNb2O6类化合物、SrTiO3类化合物、BaTiO3类化合物、BaO·R2O3·TiO2类(R：稀土类元素)、NaO·R2O3·TiO2类(R：稀土类元素)、CaO·R2O3·TiO2类(R：稀土类元素)、Li2O·R2O3·TiO2类(R：稀土类元素)、CaTiO3·R2/3TiO3(LiR)TiO3类(R：稀土类元素)等。
作为在本发明中所使用的结晶玻璃，优选使用煅烧后，将透辉石相作为主相析出的玻璃。作为所述物质，可以列举SiO2(45～60重量％)—MgO(10～30重量％)—CaO(15～35重量％)的组合结晶玻璃。而且，作为其他的结晶玻璃可举出以下例子。
·以CaO·Al2O3·SiO2为主要成分的蠕陶土类(CaO·Al2O3·2SiO2在煅烧后析出)
·以SrO·Al2O3·SiO2为主要成分的Sr长石类(SrO·Al2O3·2SiO2在煅烧后析出)
·以BaO·Al2O3·SiO2为主要成分的Ba长石类(BaO·Al2O3·2SiO2在煅烧后析出)
·以TiO2·Ln2O3为主要成分的钛酸镧类(TiO2·Ln2O3在煅烧后析出)
作为在本发明中所用的无定形玻璃，例如，可以列举如下的物质。
·以SiO2·B2O3为主要成分，相对于100重量份的SiO2，添加0.1～5重量份的Na2O的物质。
·以SiO2·B2O3为主要成分，相对于100重量份的SiO2，添加0.5～10重量份的ZrO2，0.1～5重量份的Na2O的物质。
·以SiO2·B2O3为主要成分，相对于100重量份的SiO2，添加10～25重量份的CaO的物质。
·具有SiO2(75～85重量％)—B2O3(15～25重量％)—Al2O3(0.1～5重量％)的组成的物质。
·具有SiO2(40～50重量％)—B2O3(20～30重量％)—Al2O3(15～25重量％)—CaO(4～10重量％)的组成的物质。
·SiO2(70～85重量％)—B2O3(10～25重量％)—K2O(0.5～5重量％)—Al2O3(0.01～1重量％)的组成的物质。
另外，在上述的玻璃组成中，重量％和描述的物质是将总计为100重量％的组成比例。
在本发明中，无定形玻璃还可以含有Bi，无定形玻璃中的Bi含量，以Bi2O3计，优选为30重量％或其以上，更优选为50重量％或其以上。
在本发明中，含有Bi的无定形玻璃优选还含有B，无定形玻璃中B的含量，以B2O3计，优选为5～50重量％，更优选为10～40重量％。
在本发明中，电介质陶瓷组合物中的Bi含量优选为2重量％或其以上，而且，B的含量优选为0.1～3重量％。
在本发明中，结晶玻璃和无定形玻璃的软化点可以用差热分析(DTA)测定。
本发明的层压型陶瓷零件的特征在于，所述层压型陶瓷零件由上述本发明的电介质陶瓷组合物构成的电介质层，和在该电介质层表面上形成的导体层构成的电介质生片煅烧而成的。
本发明的层压型陶瓷零件，优选构成层压型陶瓷零件的所有电介质层由上述本发明的电介质陶瓷组合物形成的电介质生片煅烧而成的。
图2是本发明的层压型陶瓷零件的立体图，图3是分解立体图。如图2和图3所示，在电介质层11上，形成了导体层12。此外，在电介质体层11中还有具有针孔13的电介质层。通过将数层这样的电介质层层压，形成了层压型陶瓷零件。
作为本发明的层压型陶瓷零件的具体实例，例如，可列举LC滤片、天线开关模块、前端模块等高频模块、光迭加模块、半导体用基板、水晶振荡器用基板、芯片LED用组件(package)、SAW装置用组件等。
根据本发明，可以得到机械强度及介电特性优良的，可在900℃左右的低温煅烧的电介质陶瓷组合物。
附图说明
图1是表示本发明的电介质陶瓷组合物的煅烧工序状态的示意图。
图2是表示一个本发明层压型陶瓷零件例子的立体图。
图3是表示一个本发明层压型陶瓷零件例子的分解立体图。
图4是表示本发明实施例的电介质陶瓷组合物煅烧后的断面的反射电子图像。
具体实施方式
以下，基于实施例，对本发明进行详细的说明。本发明并不限定于以下的实施例，在不改变要旨的情况下，可以进行适当的变化。
〔电介质陶瓷组合物的制备〕
作为结晶玻璃，使用以下(A)和(B)的玻璃。
(A)以SiO2(56重量份)—MgO(18重量份)—CaO(26重量份)作为主要成分的结晶玻璃，其软化点为800℃，结晶化点为850℃，平均粒径为2.6μm，热膨胀系数7.9为ppm/K。
(B)是以MgO·Al2O3·SiO2为主要成分，在煅烧后析出2MgO·2Al2O3·5SiO2(堇青石相)的堇青石类玻璃的结晶玻璃，其软化点为950℃，结晶化点为1050℃，平均粒径为2.7μm，热膨胀系数为9.0ppm/K。
作为无定形玻璃，使用以下(C)～(E)的玻璃。
(C)以SiO2·B2O3为主要成分，相对于对于100重量份的SiO2，添加1重量份Na2O的结晶玻璃，其软化点为566℃，平均粒径为2.7μm，热膨胀系数为8.5ppm/K。
(D)以SiO2·B2O3为主要成分，相对于100重量份的SiO2，添加5重量份的ZrO2，相对于100重量份的SiO2，添加1重量份Na2O的无定形玻璃，其软化点为750℃，平均粒径为3.4μm，热膨胀系数为6.3ppm/K。
(E)以SiO2·B2O3为主要成分，相对于100重量份的SiO2，添加20重量份CaO的无定形玻璃，其软化点为870℃，平均粒径为2.4μm，热膨胀系数为3.7ppm/K。
如表1～表3所示的那样，组合使用上述的结晶玻璃及无定形玻璃，作为陶瓷填充材料，使用Al2O3(平均粒径：1.3μm)，从而制备电介质陶瓷组合物。作为混合比例，按40重量％的结晶玻璃、10重量％的无定形玻璃及50重量％的陶瓷填充物进行混合，对于100重量份的该混合粉末，加入50重量份的异丙醇(IPA)，通过使用氧化锆制的盆或筒的球磨机对其进行60小时的湿式混合。
接下来进行干燥，挥发出溶剂成分后，添加聚乙烯醇缩丁醛(PVB)类粘合剂，再用球磨机混合24小时。
通过刮浆刀装置，将得到的浆料成形为厚50μm的生片。将此片按设定的大小切开，层压8层后，在900℃下保持2小时，进行煅烧。另外，在该煅烧工序中，进行在400℃下的脱粘合剂处理。
通过X射线衍射确定煅烧后样品的结晶结构。使用了结晶玻璃(A)的样品中，作为陶瓷填充材料的氧化铝相的峰和作为结晶玻璃的透辉石相的峰被确认为主相。
测定了各试样的抗折强度、相对密度、及介电损失。将样品加工成宽5mm，长30mm的方块状，用3点弯曲试验机(支点间距离20mm)，对抗折强度进行评价。相对密度用理论密度除以容积密度计算得到。用阻抗分析器，由1MHZ至1.8GHZ的阻抗值算出介电损失。结果如表1～表3所示。另外，在表1～表3中，本发明的范围是用粗线框所画的范围。
表1
Figure C200410104734D00091
表2
Figure C200410104734D00092
表3
如表1～表3所示，组合如本发明的范围内的结晶玻璃及无定形玻璃时，获得了高的抗折强度和相对密度。而且也降低了介电损失。在无定形玻璃的软化点附近，通过无定形玻璃发生软化流动，产生了结晶玻璃颗粒与陶瓷填充材料颗粒的再排序，由于再排序后结晶玻璃软化并结晶，促进了作为整体的致密化。
已确认，如果结晶玻璃的软化点超过900℃，煅烧会不充分，烧结后无法得到足够的密度，结果强度降低，介电损失增大。
而且，即使在结晶玻璃的软化点比无定形玻璃的软化点低的情况下，也不能获得良好特性。这被认为是由于无定形玻璃软化前，产生结晶玻璃的晶核，由于无定形玻璃的软化流动，不能充分获得粒子再排序的效果。
接下来，在上述实验中获得的优良特性的结晶玻璃(A)(软化点：800℃)和无定形玻璃(D)(软化点：750℃)的组合中，探讨了混合比例的变化。制作与上述实验相同的样品，进行与上述实验相同的抗折强度，相对密度，及介电损失的评价。评价结果如表4～表6所示。
另外，在表4～表6中，粗线框所画的范围是本发明的范围。
表4
表5
Figure C200410104734D00102
表6
Figure C200410104734D00111
如表4～表6所示，无定形玻璃为20重量％时，烧结后的密度比较高，由于无定形玻璃的成分引起的介电损失会增大。而且，结晶玻璃不足30重量％时，同样会增大介电损失。
此外，完全不含有无定形玻璃时，相对密度变低，结果还会引起抗折强度值降低。
此外，一旦结晶玻璃和无定形玻璃合计超过60重量％时，确认将引起介电损失的增大。这是由于与陶瓷填充材料相比较会导致较大损失的玻璃成分的增加。
下面，列举使用含有Bi的无定形玻璃的实施例。在电介质陶瓷组合物的制备中，使用上述的结晶玻璃(A)，作为无定形玻璃，使用以下(F)～(H)的物质。
(F)以Bi2O3(55重量％)—B2O3(35重量％)—ZnO(10重量的％)为主要成分，软化点为518℃，平均粒径为3.3μm的无定形玻璃。
(G)以Bi2O3(75重量％)—B2O3(15重量％)—ZnO(10重量％)为主要成分，软化点为469℃，平均粒径为2.9μm的无定形玻璃。
(H)以Bi2O3(60重量％)—B2O3(25重量％)—ZnO(5重量％)—SiO2(2重量％)为主要成分，软化点为536℃，平均粒径为2.6μm的无定形玻璃。
称量上述的结晶玻璃(A)和上述的无定形玻璃(F)～(H)中的1种，以及陶瓷填充材料Al2O3(平均粒径：2.6μm)，使无定形玻璃成为如表7～表9中所示的2重量％、5重量％、10重量％，结晶玻璃(A)为无定形玻璃总量的50重量％，陶瓷填充材料为50重量％，将这些混合。相对于100重量份该混合粉末，加入50重量份的异丙醇(IPA)，使用氧化锆制的筒和球构成的球磨机进行了60小时的湿式混合。
接下来进行干燥，挥发出溶剂成分后，添加聚乙烯醇缩丁醛(PVB)类粘合剂，再用球磨机混合24小时。
通过刮浆刀装置，将得到的浆料成形为厚50μm的生片。将此片按设定的大小切开，层压8层后，在900℃下保持2小时，进行煅烧。另外，在该煅烧工序中，进行在400℃下的脱粘合剂处理。
通过X射线衍射确定煅烧后样品的结晶结构，陶瓷填充物引起的氧化铝相的峰和结晶玻璃引起的透辉石相的峰被确认为主相。
测定各试样的抗折强度、相对密度、及介电损失。将样品加工成宽5mm，长30mm的方块状，用3点弯曲实验机(支点间距离20mm)，对抗折强度进行评价。相对密度用理论密度除以容积密度计算而得到。用阻抗分析器，由1MHZ至1.8GHZ的阻抗值算出介电损失。结果如表7～表9所示。另外，表中的无定形玻璃(C)是在上述的实施例中使用的不含有Bi的无定形玻璃(C)。
表7
表8
Figure C200410104734D00122
表9
Figure C200410104734D00131
使用无定形玻璃(F)～(H)的任一个时，在2～10重量％的添加量下，均能提高抗折强度和相对密度，并降低介电损失。而且，上述实施例所用的不含Bi的无定形玻璃(C)也能获得足够良好的结果，使用含Bi的无定形玻璃(F)～(H)时，尤其是相对密度较高。
此外，即使添加量较少，含Bi的无定形玻璃(F)～H)也能得到良好的结果。这是由于通过含有无定形玻璃成分Bi，煅烧时由无定形玻璃形成的液相的粘度降低，对液相的烧结促进了致密化。
〔反射电子图像的观察〕
对含有10重量％的包括Bi的无定形玻璃F的上述材料煅烧后，观察其切面的反射电子图像。图4中表示的是煅烧后试样的切面的反射电子图像。反射电子像中，在相对白的观察区域内，是由使用TEM限制视野衍射像确认的非晶形结构。而且，在该领域中，通过EDS(能量分散型X射线检测器：光束直径约1nm)进行元素分析，结果检测出了Bi和B。
在该无定形玻璃中，由于含有Bi或B，因此能够改善烧结性和机械强度。
〔层压型陶瓷零件的制备〕
在如图2所示制备的层压型陶瓷零件中，安装芯片电容器，芯片电感器，以及PIN二级管，制作高频装置。确认滤片特性时，滤片特性中的抑压度得到了改善，确认有插入损失的降低。此外，还提高了机械强度。
〔配线基板的制作〕
在使用本发明的电介质陶瓷组合物形成的厚50μm的电介质层的表面上，通过Ag糊剂，印刷期望的线路，将该电介质层层压3层后，通过煅烧，制成线路基板。结果，可以得到机械强度得到改善的线路基板。该配线基板还可以装配滤片，发送器等各种零件。

Claims (11)

1.一种电介质陶瓷组合物，所述电介质陶瓷组合物是含有结晶玻璃、无定形玻璃和陶瓷填充材料，其特征在于，上述结晶玻璃的软化点比上述无定形玻璃的软化点高，并且为900℃或其以下，所述电介质陶瓷组合物含有27重量％或其以上的结晶玻璃，不足20重量％的无定形玻璃，其中，结晶玻璃和无定形玻璃合计为60重量％或其以下，含有40重量％或其以上的陶瓷填充材料。
2.如权利要求1所述的电介质陶瓷组合物，其特征在于，上述陶瓷填充材料是由为介电常数5或其以上的材料构成。
3.如权利要求2所述的电介质陶瓷组合物，其特征在于，上述结晶玻璃煅烧后，透辉石相作为主相析出。
4.如权利要求1所述的电介质陶瓷组合物，其特征在于，上述结晶玻璃煅烧后，透辉石相作为主相析出。
5.如权利要求1～4的任一项所述的电介质陶瓷组合物，其特征在于，上述无定形玻璃含有Bi。
6.如权利要求5所述的电介质陶瓷组合物，其特征在于，上述无定形玻璃还含有B。
7.如权利要求6所述的电介质陶瓷组合物，其特征在于，煅烧后存在无定形玻璃成分，该无定形玻璃成分中含有Bi。
8.如权利要求7所述的电介质陶瓷组合物，其特征在于，上述无定形玻璃成分还含有B。
9.如权利要求5所述的电介质陶瓷组合物，其特征在于，煅烧后存在无定形玻璃成分，该无定形玻璃成分中含有Bi。
10.一种层压型陶瓷零件，其特征在于，所述层压型陶瓷零件通过将由电介质层和在该电介质层表面上形成的导体层所构成的电介质生片煅烧而得到，所述电介质层的至少1层由权利要求1～9中任一项所述的电介质陶瓷组合物构成。
11.一种层压型陶瓷零件，其特征在于，所述层压型陶瓷零件通过将由电介质层和在该电介质层表面上形成的导体层所构成的电介质生片煅烧而得到，所述电介质层的所有层都由权利要求1～9中任一项所述的电介质陶瓷组合物构成。
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