CN101410345B - 陶瓷器的制造方法、陶瓷器和电子部件 - Google Patents

陶瓷器的制造方法、陶瓷器和电子部件 Download PDF

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CN101410345B
CN101410345B CN2007800115639A CN200780011563A CN101410345B CN 101410345 B CN101410345 B CN 101410345B CN 2007800115639 A CN2007800115639 A CN 2007800115639A CN 200780011563 A CN200780011563 A CN 200780011563A CN 101410345 B CN101410345 B CN 101410345B
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powder
celsian
felspar
ceramic
porcelain
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CN101410345A (zh
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大渕武志
小田切正
井出良律
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NGK Insulators Ltd
Soshin Electric Co Ltd
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NGK Insulators Ltd
Soshin Electric Co Ltd
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Abstract

本发明涉及一种陶瓷器的制造方法，相对于陶瓷原料粉体100重量份添加0.5重量份以上、30重量份以下的六方晶系钡长石粉体制成混合物。然后，烧结该混合物制造陶瓷器时，在陶瓷器内析出针状的单斜晶钡长石。

Description

陶瓷器的制造方法、陶瓷器和电子部件
技术领域
本发明涉及一种陶瓷器的制造方法和电子部件。 
背景技术
在手机等高频率电路无线机器中，作为高频率电路过滤器例如可以使用顶部过滤器，作为送信用级间过滤器、局部过滤器、受信用级间过滤器等可以使用层压型介电体过滤器。为了制造介电体层压过滤器，制造多个构成介电体的陶瓷粉体的成型体，通过对各成型体涂上一定的导体浆在各成型体上制作一定的电极图案。然后，层压各成型体制成层压体，通过烧结这个层压体，同时烧结导体浆层和各成型体使其细密化。 
这时，电极一般使用银系导体、铜系导体、镍系导体这样的低融点金属导体，但是这些的融点例如是1100℃以下，甚至有降低到930℃左右的情况。因此，需要在比构成电极的低熔点金属的熔点更低的温度下来烧结介电体。 
为了降低杂散电容(stray capacitance)，减少延迟时间，降低内藏共振器和电容器的高频率损失，希望降低低温烧结瓷器的介电常数εr，并且增加品质系数Q。本申请人在特开2000-211969号公报中公开了具有1000℃以下的最佳烧结温度，介电常数εr为10以下，品质系数Q为2500以上的低温烧结瓷器。这个瓷器是二氧化硅-氧化铝-氧化钡系，析出强度高的钡长石相。 
另外，在特开2003-12370号公报中，通过析出硅钡石相、钡长石相和方英石相，来控制瓷器烧结时的烧结收缩，防止瓷器内开裂的发生。 
在特开2003-40668号公报记载的低温烧结瓷器中也公开了一种在瓷器内析出锌尖晶石结晶相、尖晶石结晶相、针状的钡长石结晶相等，高强度、热传导率、高杨式模量的低温烧结瓷器。 
发明内容
但是，随着电子部件的高频率化和小型化的进行，要求进一步加强陶瓷器的断裂韧性。即使在上述这样的陶瓷器中，瓷器的断裂韧性的提高仍然有上限，要求在保持其他特性的同时，实现瓷器的断裂韧性的进一步的提高。 
本发明的课题为进一步提高陶瓷器的断裂韧性。 
本发明中陶瓷器的制造方法的特征为含有，相对于陶瓷粉体100重量份，添加0.5重量份以上、30重量份以下的六方晶系钡长石粉体制成混合物的工序，和在烧结所述混合物制造陶瓷器时，在所述陶瓷器内析出单斜晶钡长石的工序。 
另外，本发明涉及一种以使用该制造方法制造为特征的陶瓷器。 
本发明关于一种以由所述瓷器构成至少一部分为特征的电子部件。 
上述的以往技术的瓷器中也在瓷器组织内析出钡长石结晶相，得到一定程度的强度提高。但是，这些钡长石相不是通过添加钡长石原料而生成的相，是通过特定的组成和制法的组合生成的相。 
本发明者在制造陶瓷器时，探讨了六方晶钡长石的添加。具体地尝试了，例如，像图1模式中所示，通过预烧主相的原料使其精制，在混合粗粉碎的低融点玻璃的阶段中添加六方晶钡长石粉体，混合后烧结。 
结果发现，通过在烧结前添加六方晶钡长石，再加入BaZn2Ti4O11、TiZn2O4、TiO2(金红石)和低融点玻璃，析出针状结晶的单斜晶钡长石。针状钡长石结晶由于能够阻止裂缝进展，所以能提高断裂韧性值。即，像图2模式所示，为了在瓷器组织内裂纹的扩展，需要移动针状结晶，移动所必须的能量抑制裂缝进展。 
但是，用本发明的制法制成的瓷器的断裂韧性的提高，与已往的析出钡长石结晶相的瓷器中的韧性提高相比有显著的增加。在讨论这个理由时，明确了以下的事情。即，像图3(a)中模式所示，相对于原料粉体4添加针状的钡长石结晶5时，针状结晶5作为一种“刺”介于其它的结晶粉体4之间，有阻碍其它粉体4烧结进行的倾向。由于像这样降低粉体的烧结性，添加针状的钡长石结晶粉体5，像图3(b)中所示，有结晶粉体1的烧结部分受阻碍且钡长石结晶粉体6的长度也变短的倾向。由于容易产生烧结不良部分，有断裂韧性降低的倾向。进一步认为，在烧结阶段，针状的钡长石结晶折断，纵横比3以下的结晶6容易残留在瓷器中。 
相对于此，如图4(a)中模式所示，相对于烧结前的瓷器原料4添加六方晶 钡长石结晶粉体7来进行烧结时，该粉体7比其它更容易收容在量多的原料粉体间4的晶界中，因此，不会妨碍其它的陶瓷器粉体4的烧结。如图4(b)中模式所示，认为随着结晶粉体4的瓷器烧结的进行，虽然粉体7变态为针状的单斜晶体2，但是在这个过程中沿着其它的结晶相1之间的细长的晶界再排列，紧密地被填充。这个结果被认为不会产生烧结的不充分部分，成为能进一步发挥单斜晶体钡长石结晶相2强度的形态。 
附图说明
图1表示有关本发明的实施方式的制造方法的流程图。 
图2表示由本发明制成的瓷器的微观构造。 
图3(a)为表示比较例中烧结前的原料混合物的模式图，图3(b)为表示图3(a)的混合物的烧结后的状态的模式图。 
图4(a)为表示本发明中烧结前的原料混合物的模式图，图4(b)为表示图4(a)的混合物的烧结后的状态的模式图。 
图5(a)为表示在实施例中制作的元件的生坯上的共振器图案的平面图，图5(b)为该元件的简化截面图。 
图6为瓷器的X射线衍射图。 
图7为由本发明制成的瓷器的电子显微镜照片。 
具体实施方式
本发明中的陶瓷器的制造方法包括，在陶瓷粉体中添加0.5重量％以上、30重量％以下的六方晶系钡长石粉体制成混合物的工序，和 
在烧结所述混合物制造陶瓷器时，在所述陶瓷器内析出针状的单斜晶钡长石的工序。 
在这里，瓷器的种类和陶瓷粉体的种类没有特别地限定，可以列举出以下组成系的瓷器：BaO-TiO2、BaO-RE2O3-TiO2(RE为镧系元素)、BaO-RE2O3-Bi2O3-TiO2(RE为镧系元素)、MgO-CaO-T2O3系。 
优选的实施方式中，陶瓷原料粉体具有BaO:9.0～26.0重量％、TiO2:30.0～75.0重量％和ZnO：0.1～38.0重量％的陶瓷组成。在由这样的原料粉体制成的钛酸钡(锌)系瓷器中，析出单斜晶钡长石的瓷器发现具有特别优异的断裂韧性。
进一步优选的实施方式中，陶瓷原料粉体中BaO、TiO2和ZnO的合计量为100重量份时，进一步含有Al2O3：0.7～15.0重量份，SiO2：0.1～15.0重量份，MnO：0.1～5.5重量份和B2O3：0.1～20.0重量份。 
钡长石结晶相的高温相为六方晶系，低温相变为单斜晶体系。因此，除了瓷器原料的主相，还添加玻璃粉体到六方晶钡长石中，在比较低温下烧结时，能够推断出低温相的单斜晶体变得容易析出。 
另外，除了瓷器原料粉体和六方晶钡长石粉体，优选添加玻璃粉体。这时，作为玻璃粉体有以下的示例：ZnO-SiO2-B2O3、SiO2-B2O3、BaO-Al2O3-SiO2-B2O3、BaO-Bi2O3-B2O3、Li2O-R2O3-SiO2-B2O3、Li2O-RO-SiO2-B2O3(R为碱土类金属)。 
本发明的制法中，在陶瓷粉体中添加0.5重量份以上、30重量份以下的六方晶系钡长石粉体。钡长石粉体的重量比率以原料粉体的合计量为100重量份计算。在这里，通过使六方晶系钡长石粉体的比率达到0.5重量份以上，能够促进瓷器中的单斜晶钡长石结晶的析出，因此，可以进一步提高瓷器中的断裂韧性。由这个观点出发，六方晶系钡长石粉体的添加量进一步优选为2.0重量份以上。 
另外，如果六方晶系钡长石粉体的添加量超过30重量份，烧结性下降，瓷器中的缺陷增加。因此，六方晶系钡长石粉体的添加量为30重量份以下。由这个观点出发，其添加量进一步优选25重量份以下。 
相对于构成瓷器的各金属原料的混合物可以添加六方晶钡长石粉体。或者，混合六方晶钡长石粉体以外的各氧化物，进行预烧制造预烧物，粉碎预烧物制成预烧粉体，相对于预烧粉体添加六方晶钡长石粉体和玻璃粉体后混合，烧结该混合物。 
钡长石粉体添加时，可以进一步添加在瓷器制造时通常使用的添加剂。作为这样的添加剂，可以举出部分稳定化氧化锆和氧化铝。 
在瓷器中析出的针状钡长石结晶相的长度没有限定，通常为1.6～3.0μm。另外，该钡长石结晶相的直径通常为0.1～0.8μm，纵横比通常为2.0～30。 
本发明的陶瓷器中，通过BaO的比率为9.0～26.0重量％，瓷器的气孔率变得显著降低，断裂韧性提高，另外能够抑制强介电体层的析出。
通过TiO2的比率为30.0～75.0重量％，可以明显地降低瓷器的气孔率，提高断裂韧性，抑制开裂。 
通过ZnO的比率为0.1～38.0重量％，可以明显地降低瓷器的气孔率，提高断裂韧性，抑制开裂。 
本发明中适宜地陶瓷组成中，可以进一步使Al2O3的比率为0.7～15.0重量份。但是，BaO、TiO2和ZnO的合计量为100重量份。通过添加这样的Al2O3，可以控制瓷器的烧结性。 
本发明中适宜地陶瓷组成中，可以进一步使SiO2的比率为0.1～15.0重量％。但是，BaO、TiO2和ZnO的合计量为100重量份。通过添加这样的SiO2，可以控制瓷器的烧结性。 
本发明中适宜地陶瓷组成中，可以进一步使MnO的比率为0.1～5.5重量％。但是，BaO和ZnO的合计量为100重量份。通过添加这样的MnO，可以控制瓷器的烧结性。 
本发明中适宜地陶瓷组成中，可以进一步使B2O3的比率为0.1～20.0重量％。但是，BaO、TiO2和ZnO的合计量为100重量份。通过添加这样的B2O3，可以控制瓷器的烧结性。 
本发明中X射线衍射图和峰强度用以下的条件来测定。 
X射线衍射装置名：RIGAKU制「Multi Flex」， 
管球：Cu管， 
电压：50kV， 
管电流：30mA， 
单色器：入射端Ge发散缝隙:1/2deg， 
散乱缝隙：1/2deg， 
受光缝隙：0.15mm， 
步长：0.02deg， 
计数时间：2.0sec。 
本发明的瓷器可以含有在各金属原料中不可避免的杂质。另外，也可以含有上述成分以外的氧化物或者金属成分。作为这样的氧化物或者金属成分有例如MgO、CaO、SrO、Y2O3、V2O3、CoO、NiO、Nd2O3、Sm2O3、La2O3、CuO、 Ag、Cu、Ni、Pd。 
作为本发明对象的电子部件没有特别的限定，可以举出例如层压介电体过滤器、多层配线基板、介电体天线、介电体耦合器、介电体复合组件。 
本发明的电子部件中优选相对于电子部件的其他部件连接陶瓷器。其它的部件没有限定，优选为介电体层、磁体层、压电体层或者金属电极。 
电子部件中可以使用的金属电极没有限定，但是优选银电极、铜电极、镍电极或者他们的合金或者由它们的混合物组成的电极，更优选银、银合金、银和其它金属和其混合物组成的电极，特别优选银电极。 
另外，在金属电极上可以设置镀层和/或软焊料层。镀层的成分可以列举出Ni和Sn。软焊料层的成分可以列举出Sn-Pb、Sn-Pb-Ag、Sn-Pb-Sb、Sn-Pb-In-Sb-Ag、Sn-Pb-Ag-Cu、Sn-Zn-In、Sn-Ag、Sn-Ag-Bi-Cu、Sn-Ag-Cu、Sn-Cu、Sn-Sb-Ag-Cu、Sn。 
本发明的电子部件中可以使本发明的低温烧结瓷器与介电常数εr为10-150的其它的低温烧结瓷器一体化。 
这样的瓷器的组成系没有限定，但是优选以下的组成系：BaO-TiO2-ZnO-SiO2-B2O3、BaO-TiO2-Bi2O3-Nd2O3-ZnO-SiO2-B2O3、BaO-TiO2-Bi2O3-La2O3-Sm2O3-ZnO-SiO2-B2O3、MgO-CaO-TiO2-ZnO-Al2O3-SiO2-B2O3。 
构成磁体层的磁体可以举出以下的物质：MnO-ZnO-Fe2O3-CuO、MnO-ZnO-Fe2O3-CuO-SiO2、MnO-ZnO-Fe2O3-CuO Ta2O5、MnO-ZnO-Fe2O3-CuO-SiO2-Ta2O5、NiO-ZnO-Fe2O3、MnO-ZnO-Fe2O3、MnO-ZnO-Fe2O3-Bi2O3-MoO3、NiO-CuO-ZnO。 
构成压电体层的压电体可以举出以下的物质：PdO-ZrO2-TiO2、PdO-ZrO2-TiO2-Sb2O3、K2O-Na2O-Li2O-Nb2O3-Ta2O3-Bi2O3、PbO-CoO-Nb2O3-ZrO2-Ti2O、PbO-MgO-Nb2O3-Yb2O3-TiO2-ZrO2、BaO-TiO2。 
在制造本发明的低温烧结瓷器时，优选在规定比率下混合各金属成分的原料制成混合粉体，在850-1200℃预烧混合粉体，粉碎预烧体，制成陶瓷粉体。然后，优选使用陶瓷粉体、低融点玻璃粉体和六方晶钡长石粉体，制造生坯，在850-930℃烧结生坯。作为各金属成分的原料可以使用各金属的氧化物、硝酸盐、碳酸盐、硫酸盐等。
实施例 
试验编号1-10 
陶瓷粉体的制造 
称量碳酸钡、氧化钛和氧化锌的各粉体为表1所示的规定组成。称量氧化铝和氧化锰的各粉体各自为0.5重量份和0.8重量份后添加。湿式混合这些混合物后，在1250℃下预烧该混合粉体制成预烧体。为了测试预烧物的结晶相和它的结晶性，进行粉体X射线衍射测定时，得到以下的结晶相： 
[0067] BaZn2.03Ti3.93O10.89相(ICSD No.81-2380) 
[0068] TiZn2O4相(ICSD No.77-0014) 
TiO2(金红石)相(ICSD No.73-1765) 
接下来，在球磨机中粉碎该预烧粉体至一定粒度，干燥粉体，制成陶瓷原料粉体。 
玻璃粉体的制造 
称量SiO2、ZnO和B2O3各粉体，干式混合，在白金坩埚中熔融混合粉体，在水中投入熔融物后迅速冷却，制成块状的玻璃。湿式粉碎该玻璃后制成低融点的玻璃粉体。 
六方晶钡长石粉体的制造 
根据钡长石的组成比率湿式混合碳酸钡、氧化铝和氧化硅各粉体，在1350℃预烧制成六方晶钡长石预烧物。粗粉碎后制成预烧粉体。制成的预烧粉体的X射线衍射的谱峰与六方晶钡长石一致。 
烧结 
上述的陶瓷原料粉体、玻璃粉体和六方晶钡长石粉体一起微粉碎。另一方面，混合有机溶剂、粘合剂、增塑剂和分散剂，添加到微粉碎的混合粉体中，使用氧化铝罐和氧化铝球混合，制成浆，干燥浆得到造粒粉体。用模具压缩机将得到的造粒粉体成型为一定的形状，在920℃下烧结制成烧结体瓷器。 
气孔率的测定 
制成的烧结体的气孔率用阿基米德法测定。 
X射线衍射峰的测定 
对各瓷器试料在前述的条件下测定X射线衍射峰。结果确认了以下的结 晶相。 
断裂韧性值 
前述陶瓷粉体、玻璃粉体和六方晶钡长石粉体和有机粘合剂、增塑剂、分散剂和有机溶剂一起用氧化铝罐和氧化铝球湿式混合，制成生坯成型用浆。用该浆通过刮刀装置成型为厚为0.03～2mm的各生坯。层压一定张数的各生坯通过CIP法制成层压体，用切粒机切断成11mm×8mm×3mm的形状，通过在920℃烧结制成烧结体。然后，洗净烧结体，在镍中进行电镀，然后在锡中性槽中进行电镀，洗净制成的试料。对这个试料用JIS-R-1607压头压入法(IF法)测定断裂韧性值。 
断裂发生数 
和上述同样地成型为厚为0.03～2mm的各生坯。由Ag-Pt(Pt1重量％)浆在各生坯上通过丝网印刷形成作为模型图案的图5(a)和(b)的共振器电极图案11，层压一定张数的各生坯10、12成为图5(b)的层压构造，通过CIP法制成层压体，烧结后的尺寸用切粒机切断成3.2mm×2.5mm×1.8mm，印刷外装电极后，在920℃下烧结。制成的烧结体暴露在以下的热冲击和高湿度条件下，然后用超声波探伤法评价裂纹的有无。裂纹有无的确认是用超声波探伤装置(日立建机株式会社制「マイスコ—プ」)由从开裂的部分起的B超反射的画像数据来判断。测定各自的1000个试料，次品的发生数表示在表中。 
热冲击条件 
一次循环为-55℃～+125℃，1次循环的时间为1个小时，进行33次循环。高湿度条件 
85℃、85％RH、240小时 
如果六方晶钡长石的添加量如果为30重量份以下，开裂的发生率变高，断裂韧性值上升。在本发明的范围内断裂韧性值高，也几乎不发生断裂。 
另外，对试验编号2-9的各例中的试料进行上述的X射线衍射试验时，确认到以下的结晶相。 
BaZn2Ti4O11相(ICSD No.81-2380) 
TiZn2O4相(ICSD No.77-0014) 
TiO2(金红石)相(ICSD No.73-1765)
单斜晶钡长石相(ICSD No.74-1677) 
图6为无添加六方晶钡长石粉体情况的瓷器和添加六方晶钡长石粉体(10.0重量份)的瓷器的X射线衍射图。由添加六方晶钡长石粉体制成的瓷器，确认到单斜晶钡长石的衍射峰。 
另外，图7为有关添加六方晶钡长石粉体(10.0重量份)的瓷器的照片。发现沿晶界析出多个针状的结晶相。例如，确认有关4个地方的针状结晶时，长、直径和纵横比为以下。 
长2.1μm　　　直径  0.4μm　　　纵横比  5.3 
长1.4μm　　　直径  0.4μm　　　纵横比  3.5 
长1.6μm　　　直径  0.4μm　　　纵横比  4.0 
长1.3μm　　　直径  0.4μm　　　纵横比  3.3 
试验号11-18 
同试验编号1-10同样地制造表2所示的各瓷器。结果发现，在陶瓷原料粉体中添加30重量份以下的六方晶钡长石，在瓷器中析出单斜晶体钡长石的情况下，断裂韧性值显著地提高，防止开裂。但是，如果氧化钡超过30重量份，在瓷器中生成强介电体。 
试验编号19-28 
同试验号编1-10同样地制造表3所示的各瓷器。结果发现，在陶瓷原料粉体中添加30重量份以下的六方晶钡长石，在瓷器中析出单斜晶钡长石的情况下，断裂韧性值显著地提高，防止开裂。 
试验编号29-37 
同试验编号1-10同样地制造表4所示的各瓷器。结果发现，在陶瓷原料粉体中添加30重量份以下的六方晶钡长石，在瓷器中析出单斜晶钡长石的情况下，断裂韧性值显著地提高，防止开裂。 
试验编号38-45 
同试验编号1-10同样地制造表5所示的各瓷器。结果发现，在陶瓷原料粉体中添加30重量份以下的六方晶钡长石，在瓷器中析出单斜晶钡长石的情况下，断裂韧性值显著地提高，防止开裂。 
虽然说明了本发明的特定的实施方式，但是本发明不受这些特定的实施方式限定，只要不离开权利要求的范围，可以实施进行种种的变更或改变。
Figure G2007800115639D00111
Figure G2007800115639D00121
Figure G2007800115639D00131
Figure G2007800115639D00141

Claims (5)

1.一种陶瓷器的制造方法，其特征在于，包括，相对于陶瓷原料粉体100重量份，添加0.5重量份以上、30重量份以下的六方晶系钡长石粉体来制造混合物的工序，和，
在烧结所述混合物制造陶瓷器时，在所述陶瓷器内析出单斜晶钡长石的工序。
2.根据权利要求1所述的陶瓷器的制造方法，其特征在于，向所述混合物添加烧结助剂。
3.根据权利要求1或2所述的陶瓷器的制造方法，其特征在于，所述烧结时的温度为850℃以上、1100℃以下。
4.根据权利要求1～3中任一项所述的陶瓷器的制造方法，其特征在于，所述陶瓷原料粉体具有BaO：9.0～26.0重量％、TiO2：30.0～75.0重量％和ZnO：0.1～38.0重量％的陶瓷组成。
5.根据权利要求4中所述的陶瓷器的制造方法，其中，所述陶瓷原料粉体中BaO、TiO2和ZnO的合计量为100重量份时，进一步含有Al2O3：0.7～15.0重量份、SiO2：0.1～15.0重量份、MnO：0.1～5.5重量份和B2O3：0.1～20.0重量份。
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