CN1289427C - 介电陶瓷组合物和介电陶瓷 - Google Patents

介电陶瓷组合物和介电陶瓷 Download PDF

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CN1289427C
CN1289427C CNB03103411XA CN03103411A CN1289427C CN 1289427 C CN1289427 C CN 1289427C CN B03103411X A CNB03103411X A CN B03103411XA CN 03103411 A CN03103411 A CN 03103411A CN 1289427 C CN1289427 C CN 1289427C
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powder
weight
dielectric ceramic
diopside
temperature
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CN1435390A (zh
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古濑辰治
平原诚一郎
中泽秀司
大出泰
儿嶋知将
关根史明
牧野浩
米仓学
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Kyocera Corp
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Kyocera Corp
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Priority claimed from JP2002123057A external-priority patent/JP3898560B2/ja
Priority claimed from JP2002137578A external-priority patent/JP2003286074A/ja
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Abstract

本发明提供一种介电陶瓷组合物，该组合物包含：30～90%重量的能够沉积透辉石晶体的结晶玻璃粉，1～40%重量的钛酸钙粉、钛酸锶粉或其混合粉，和0～60%重量的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末，以及焙烧该组合物得到的介电陶瓷。

Description

介电陶瓷组合物和介电陶瓷
技术领域
本发明涉及一种介电陶瓷组合物和介电陶瓷，更具体而言，涉及这样的一种介电陶瓷组合物和介电陶瓷，它们在诸如微波或毫米波的高频区表现出8～22的相对介电常数，与常规的玻璃陶瓷相比，还具有较高的机械强度和高精度的温度系数。
背景技术
迄今为止，介电陶瓷已经被广泛应用于介电谐振器、MIC(麦克风)和用于高频应用领域，例如微波或毫米波的波导管的介电底基材料。随着近年来包括手机的移动通讯的发展和传播，对用作电子线路板和电子部件材料的介电陶瓷的需求已经与日俱增。
已经研发出了由玻璃制成的所谓的玻璃陶瓷，这种玻璃陶瓷可以和诸如银或铜的高导电金属一起焙烧，或者玻璃和陶瓷的复合材料作为电子线路板和电子部件的介电陶瓷组合物。
例如，未审的专利申请(Kokai)No.2001-348268叙述了一种含SiO2，CaO，MgO，B2O3和Al2O3的介电陶瓷组合物，该组合物可以在1000℃或更低的温度下焙烧，并可用于高频部件中。
尽管未审专利申请(Kokai)No.2001-348268中所述的介电陶瓷组合物表现出了低的介电损失，但是因为这种介电陶瓷共振频率的温度系数大，增加了静电容的温度系数，因此不能获得所需的与操作环境相符的导电特性。因为其机械强度低，很容易因使用这种介电陶瓷的电子设备的下落碰撞而发生破裂。
发明内容
发明概述
本发明的一个主要目的是提供适用于高频部件，并可控制高精度温度特性的高强度介电陶瓷组合物和高强度介电陶瓷。
本发明的另一个目的是提供一种介电陶瓷组合物和介电陶瓷，其可以防止底基在和导体一起焙烧时的褪色或者给底基染色，因而可以减少不良外观的比率。
本发明是基于这样一种发现而完成的，即通过使用一种介电陶瓷组合物，该组合物含能够沉积透辉石晶体的结晶玻璃，钛酸钙和/或钛酸锶，以及至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的物质，可以改善共振频率的温度特性，并可以实现对所需介电常数和高强度的控制。本发明的介电陶瓷组合物包含至少一种能够沉积透辉石晶体的结晶玻璃粉，以及钛酸钙和/或粉末状钛酸锶。
具体而言，本发明的介电陶瓷组合物包含：
(1)30～90％重量的能够沉积透辉石晶体的结晶玻璃粉，
(2)1～40％重量的钛酸钙粉，钛酸锶粉或混合粉末，以及
(3)0～60％重量的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的物质。
通过使用各种粉末和这种组合物的混合物，可以改善焙烧后所形成的介电陶瓷共振频率的温度特性，并可以实现对所需介电常数和高强度的控制。
为了增强介电陶瓷的机械强度，并改善诸如共振频率的温度系数之类的介电特性，还优选用于介电陶瓷组合物的能够沉积透辉石晶体的结晶玻璃，钛酸钙粉末，钛酸锶粉末，或者钛酸钙粉和钛酸锶粉混合粉的平均颗粒大小为3μm或更小。
本发明其他的介电陶瓷组合物包含：
[I]100重量份的混合粉末，其包含：(1)30～90％重量的能够沉积透辉石晶体的结晶玻璃粉，(2)1～40％重量的钛酸钙粉，钛酸锶粉或其混合粉末，和(3)0～60％重量的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的物质，以及
[II]0.1～2.0重量份的至少一种选自Fe2O3，Cr2O3，ZnO，CuO，Ag2O，Co3O4，MnO2，CeO2和R2O3(R表示稀土元素)的粉末(色调改进剂)。
通过使用各种粉末和这种组合物的混合物，可以改善焙烧后所形成的介电陶瓷的共振频率的温度特性，并可以实现对所需介电常数和高强度的控制。而且，还可以防止底基在和导体一起焙烧时的褪色或者给底基染色，因而可以减少不良外观的比率。
可以通过在850～1050℃的温度下焙烧介电陶瓷组合物混合物的预成型坯(料坯)来获得本发明的介电陶瓷，其相对介电常数εr为8～22，三点弯曲强度为250MPa或更大，而共振频率的温度系数为0±60×10-6/℃。
因此，在用于MIC和电子部件的介电底基材料中，当和以Ag或Cu为主要成分的导体一起焙烧时，可以防止发生弯曲和变形，还可以设计出高功能的高频电路部件。而且，当使用加入了色调改进剂的介电陶瓷组合物时，可以防止因导体的还原作用引起的褪色或者对底基的染色。
在本发明的介电陶瓷中，优选静电容的温度系数为0±150×10-6/℃。由此，可以抑制因温度改变而导致的静电容的变化，并且可以高精度地控制介电陶瓷的温度特性。
此外，在焙烧后的陶瓷中，优选至少透辉石和/或透辉石固溶体以及钛酸钙和/或钛酸锶是以晶相形式共存的。如上所述，通过使能够改变介电陶瓷强度和温度系数的晶相共存于介电陶瓷中，可以增强介电陶瓷的机械强度，并可以容易地控制相对介电常数和温度系数。
优选焙烧后的陶瓷在室温～400℃下测量的热膨胀系数为8×10-6/℃或更高。因此，可以使介电陶瓷的热膨胀系数接近于用于母板的玻璃环氧树脂的热膨胀系数，从而可以改善安装的耐热冲击性。
附图说明
图1是本发明介电陶瓷实施例1中1号样品的粉末X-射线衍射图。
发明详述
本发明的介电陶瓷组合物中包含能够沉积透辉石晶体的结晶玻璃，钛酸钙粉，钛酸锶粉，或其混合粉末，还有至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末(填料成分)，这一点很重要。
优选使用透辉石晶体，因为透辉石的介电常数相对较大，介电损失较小，并且在高频下具有高强度。
使用钛酸钙和/或钛酸锶是为了补偿沉积在介电陶瓷组合物中透辉石晶体的共振频率的温度系数。单独使用透辉石晶体时，共振频率的温度系数表现出负向特征，而单独使用钛酸钙和/或钛酸锶时，共振频率的温度系数表现出正向特征。因此，优选使用透辉石晶体来控制共振频率的温度系数。
优选结合使用诸如Al2O3的填料成分，以改善介电陶瓷的机械强度，并将温度特性补偿至钛酸钙的数量。
为了组成本发明的介电陶瓷组合物，介电陶瓷组合物中包含30～90％重量的能够沉积透辉石晶体的结晶玻璃，1～40％重量的钛酸钙粉，以及0～60％重量的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末是很重要的。
出于如下原因，将能够沉积透辉石晶体的结晶玻璃粉的数量限定在30～90％重量的范围内，即，结晶玻璃粉的数量处于上述范围时，可以在850～1050℃的温度下形成高密度的介电陶瓷，还可以和以Ag或Cu为主要成分的导体一起焙烧。当结晶玻璃粉的数量少于30％重量时，该组合物在低于1050℃的温度下无法烧结，也不可能和以Ag或Cu为主要成分的导体一起焙烧。另一方面，当其数量超过90％重量时，就会降低机械强度，并难以在玻璃焙烧软化时维持形状，导致接线底基尺寸的精确度差。因此，为了维持可烧结性，高强度和尺寸的高精度，更优选结晶玻璃粉的数量为40～80％重量。
优选能够沉积透辉石晶体的结晶玻璃粉组成为30～55％重量的SiO2，10～35％重量的MgO和24～40％重量的CaO。Al2O3可以单独或者和ZnO一起包含于结晶玻璃粉中。所需Al2O3的数量为4.5～15％重量。
除了透辉石以外，优选选自锌黄长石，钡长石，堇青石，钙长石，锌尖晶石，硅锌矿，尖晶石和富铝红柱石的至少一种物质从玻璃粉中沉积，因为这样可以得到高强度。
钛酸钙粉的数量限制在1～40％重量范围内，理由如下：在25～85℃的温度范围内，透辉石晶体共振频率的温度系数τf为-63×10-6/℃，表现出负向特性，钛酸钙粉所表现出的共振频率的温度系数τf为840×10-6/℃，这两种物质共存于介电陶瓷中，都可以补偿共振频率的温度系数，并将其控制在0±60×10-6/℃的范围内。
当钛酸钙粉的数量少于1％重量时，难以改善介电陶瓷的相对介电常数，也难以将共振频率的温度系数控制在0±60×10-6/℃的范围内。另一方面，钛酸钙量超过40％重量时，共振频率的温度系数增加至正向，难以在维持其可烧结性的同时还将共振频率的温度系数控制在0±60×10-6/℃的范围内。因此，为了高精度地控制温度，更优选钛酸钙粉的数量为3～30％重量。此处，控制共振频率的温度系数在0±60×10-6/℃的范围内是指温度系数的绝对值为60×10-6/℃或更小。
用于取代钛酸钙粉的钛酸锶粉的数量限定为1～40％重量，其理由如下：在25～85℃的温度区间，透辉石晶体共振频率的温度系数τf为-63×10-6/℃，表现出负向特性，钛酸锶粉表现出的共振频率的温度系数τf为1670×10-6/℃，这两种物质共存于介电陶瓷中，都可以补偿共振频率的温度系数，并将其控制在0±60×10-6/℃。
当钛酸锶粉的数量少于1％重量时，难以改善介电陶瓷的相对介电常数，也难以将共振频率的温度系数控制在0±60×10-6/℃。另一方面，钛酸锶数量超过40％重量时，共振频率的温度系数增加至正向，难以在维持其可烧结性的同时还将共振频率的温度系数控制在0±60×10-6/℃。因此，为了高精度地控制温度，更优选钛酸锶粉的数量为3～30％重量。此处，控制共振频率的温度系数在0±60×10-6/℃是指温度系数的绝对值为60×10-6/℃或更小。
当用钛酸钙和钛酸锶混合粉代替钛酸钙或钛酸锶时，混合粉的数量限定在1～40％重量，理由如下：在25～85℃的温度区间，透辉石晶体共振频率的温度系数τf为-63×10-6/℃，表现出负向特性，而混合粉末在钛酸钙和钛酸锶两相共存的状态下，表现出的共振频率的温度系数τf为840×10-6/℃～1670×10-6/℃，这两种物质共存于介电陶瓷中，都可以补偿共振频率的温度系数，并将其控制在0±60×10-6/℃。
当钛酸钙和钛酸锶混合粉的数量少于1％重量时，难以改善介电陶瓷的相对介电常数，也难以将共振频率的温度系数控制在0±60×10-6/℃。另一方面，混合粉数量超过40％重量时，共振频率的温度系数增加至正向，难以在维持其可烧结性的同时还将共振频率的温度系数控制在0±60×10-6/℃。因此，为了高精度地控制温度，更优选钛酸钙和钛酸锶混合粉的数量为3～30％重量。
此处，控制共振频率的温度系数在0±60×10-6/℃是指温度系数的绝对值为60×10-6/℃或更小。
至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末作为填料组分，其数量限定在0～60％重量，理由如下：当其数量超过60％重量时，在1050℃或更低的温度下不能烧结。具体而言，从可烧结性考虑，优选其数量为50％重量或更小。优选选择并制备如下复合物作为本发明所用的填料组分，来控制共振频率的温度系数接近于零：钛酸钙和/或钛酸锶，其共振频率的温度系数表现出正向特性；TiO2和BaTi4O9，其温度系数表现出正向特性；以及Al2O3，ZrO2，MgTiO3，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3，其共振频率的温度系数表现为负向特性。更优选填料组分的量为0.5～30％重量。
除了上述化合物以外，该组合物可以包含V，Cr，Mo，W，Mn，Co，Ni，Cu，Ag，Ru，Cd及其氧化物，数量为10％重量或更小，只要这些物质在和导体一起焙烧时不会出现底基的弯曲或变形，并能维持其强度就行。
为了控制可烧结性、陶瓷的高强度和共振频率的温度系数，优选用作填料组分的粉末的平均颗粒大小为1～3.5μm，而为了改善在能够沉积透辉石晶体的结晶玻璃粉、钛酸钙粉或钛酸锶粉中的分散性，更优选其大小为1.2～3μm。
下面描述用本发明的组合物制造介电陶瓷的方法。首先，制备平均颗粒大小为1～3μm的玻璃粉，平均颗粒大小各为1～3μm的钛酸钙粉和/或钛酸锶粉，和至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末作为填料组分。
优选能够沉积透辉石晶体的结晶玻璃粉、钛酸钙粉或钛酸锶粉的平均颗粒大小为3μm或更小，因为这样可以在850～1050℃的温度下焙烧获得高密度的介电陶瓷，更优选颗粒大小为1.5～2.5μm，因为这样能够补偿共振频率的温度系数，并得到高强度。
至于钛酸钙粉和/或钛酸锶粉和填料组分的组合，优选选择共振频率的温度系数表现出正向特性的钛酸钙和/或钛酸锶的组合，温度系数显示为正向特性的(TiO2和BaTi4O9)组，和共振频率温度系数表现出负向特性的(Al2O3，ZrO2，MgTiO3，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3)组，并制备出来以控制共振频率的温度系数接近于零。然后，将这些生粉称重，并按上述比例在使用ZrO2球的球磨机中混合，获得颗粒大小为2.0μm或更小的磨碎的混合物。
采用各种已知的成型方法，例如冲压法，刮板法，注射成型法或带式成型(tape forming)法，将所得的混合粉制成预定形状的预成型坯。这些方法中，特别优选用刮板法和带式成型法来制备薄板制品。
将所得预成型坯在诸如空气的氧化性环境或者诸如氮气的非氧化性环境中，在850～1050℃焙烧0.5～2小时，得到介电陶瓷。
可以使用诸如氢氧化物，碳酸盐和硝酸盐之类的、在焙烧时能够产生氧化物的金属盐作为生粉。本发明的介电陶瓷组合物可以包含一些不可避免的杂质，例如Fe，Hf，Sn，Nb，Na和K，只要这些杂质不对陶瓷的特性和可烧结性产生负面影响就行。
为了控制温度特性，特别优选透辉石和/或从玻璃粉中沉积出的透辉石固溶体和钛酸钙和/或钛酸锶颗粒共存于介电陶瓷中。当透辉石晶体和钛酸钙和/或钛酸锶残留在陶瓷中时，会给介电陶瓷带来高强度。
图1是介电陶瓷实施例的粉末X-射线衍射图，该介电陶瓷是用钛酸钙作为本发明的介电陶瓷组合物，Al2O3作为填料，并焙烧该组合物而获得的。如图1所示，存在清晰的表示透辉石晶体、钛酸钙和加入作为填料组分的Al2O3的晶相的X-射线衍射峰。这一事实很清楚地表明透辉石晶体、钛酸钙和Al2O3组分共存于介电陶瓷中。其它杂相也可以共存，只要该杂相是不显著影响介电陶瓷强度和介电特性的晶相。电子显微镜观察显示颗粒状CaTiO3和Al2O3是均匀分散的。
当用钛酸锶粉或钛酸钙粉和钛酸锶粉混合物取代钛酸钙粉作为填料时，也得到相同的趋势。
在本发明的含有上述组成的介电陶瓷中，εr可以在8～22的范围内变化，可以将陶瓷的三点弯曲强度控制在250MPa或更大，可以将共振频率的温度系数控制在0±60×10-6/℃，(更)特别地，0±40×10-6/℃，可以将静电容的温度系数控制在0±150×10-6/℃，特别是0±70×10-6/℃。同样，可以将焙烧温度控制在850～1050℃，该焙烧温度下允许组合物和以Ag或Cu作为主要组分的导体一起焙烧。因此，即使是和导体一起焙烧的情况下，也可以抑制出现弯曲或变形现象。
本发明的介电陶瓷中，在室温～400℃的温度范围内测得的热膨胀系数优选为8×10-6/℃或更大，更优选为8.5×10-6～9.8×10-6/℃。
为了组成本发明其它的介电陶瓷，在100重量份的含如下成分的混合粉(I)中进一步加入0.1～2.0重量份的至少一种选自Fe2O3，Cr2O3，ZnO，CuO，Ag2O，Co3O4，MnO2，CeO2和R2O3(R表示稀土元素)的粉末(II)：30～90％重量的能够沉积透辉石晶体的结晶玻璃，总共1～40％重量的钛酸钙粉和/或钛酸锶粉，以及0～60％重量的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末。
至少一种选自Fe2O3，Cr2O3，ZnO，CuO，Ag2O，Co3O4，MnO2，CeO2和R2O3(R表示稀土元素)的粉末(II)的加入量，以混合粉(I)的重量为100份计，为0.1～2.0重量份，理由如下：这些粉末是作为调色剂加入的，为的是通过防止因和导体一起焙烧产生的还原作用造成的透辉石晶相的褪色来抑制底基的染色不均匀现象，或者染色底基，同时抑制机械强度的降低和变化。当粉末(II)的数量超过2.0重量份时，机械强度会显著降低。而当其数量不足0.1重量份时，则没有防止褪色或者染色的作用。为了防止褪色或通过维持高机械强度来控制底基，更优选其数量为0.1～1.0重量份。为了更有效地发挥上述作用，优选这些氧化物的颗粒大小为1.0μm或更小。
当采用本发明的介电陶瓷组合物来制造介电陶瓷时，首先，制备包含如下成分的混合粉作为填料组分：平均颗粒大小为2.0μm的透辉石玻璃粉，平均颗粒大小各为2.0μm的钛酸钙粉和/或钛酸锶粉，和至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末；还有，至少一种选自Fe2O3，Cr2O3，ZnO，CuO，Ag2O，Co3O4，MnO2，CeO2和R2O3(R表示稀土元素)的粉末作为调色剂。然后，按上述比例混合所得的粉末，并按上述相同的方法成型然后焙烧，以获得本发明的介电陶瓷。
具体实施方式
实施例1
首先，用如下玻璃料A和B作为玻璃料，该玻璃料是能够沉积透辉石晶体、平均颗粒大小为2μm的结晶玻璃粉。玻璃料A：45重量％SiO2-25重量％CaO-15重量％MgO-10重量％ZnO-5重量％Al2O3玻璃料B：49重量％SiO2-28重量％CaO-18重量％MgO-5重量％Al2O3
使用平均颗粒大小为2μm、99％或更高纯度的CaTiO3粉末和平均颗粒大小各为2μm的Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3以及CaZrO3作为填料。分别称重各个组分，并按表1所示的比例和水混合，在使用ZrO2球的球磨机中湿化处理20小时，得到颗粒大小为1.5μm或更小的磨碎的混合物。
作为比较例，使用不能沉积透辉石晶体的结晶玻璃粉(玻璃料C：50重量％的SiO2-40重量％的BaO-10重量％的Al2O3)。
将磨碎的混合物制成圆柱形预成型坯，大小为5mm×4mm×50mm，作为在100MPa压力下评估弯曲强度的样品，在表1所示的最大温度条件下焙烧1小时得到大小为4mm×3mm×40mm的样品。在室温下对该样品进行三点弯曲强度测量，条件是：十字头速度为0.5mm/min，低支架之间的距离为30mm。采用测量热膨胀系数的仪器测量热膨胀系数，结果见表2。
同样，将上述磨碎的混合物制成直径10mm、高8mm的圆柱形预成型坯样品，用来在100MPa压力下进行介电特性的评估，在表1所示的最大温度条件下焙烧1小时，得到直径8mm、高6mm的样品。
在介电特性的评估方面，用介电圆柱体谐振器法在9～15GHz下测量样品的相对介电常数εr，在-40～85℃的温度范围内测量共振频率的温度系数τf。结果见表2。表中的τf[×10-6/℃]是在25～85℃的温度下测得的数值，用如下等式表示：
τf＝(1/f25℃)(f85℃-f25℃)/(60℃)×106
其中f25℃表示25℃时的共振频率，f85℃表示85℃时的共振频率。表中的TCC为静电容的温度系数，用τf表示，热膨胀系数α是根据如下公式计算的：
TCC＝-2(α+τf)
其中热膨胀系数α是在室温～400℃的温度范围内测得的数值。
介电陶瓷中的晶相是通过X-射线衍射来鉴别的。结果见表2。
表1
序号   玻璃 CT**(重量％)   填料组成(重量.％)*** 焙烧温度℃
组分 重量％ AL Ti Zr MT BT LT NT CN SZ CZ
  12345678*910111213141516171819202122*232425*26*27*28*29*30   AAAAAAAAABBBBBBBBBBBBBBBBBBCBB   607065687275656060607080625274645458534850459590302070603040   10105735131509910886667772040522040010545   291929242420105403020929392030403540452000840403030655   110000000100000000000000000000   001100000000100000000000000000   000010000001000000000000000000   000000100000000000000000000000   000000100000000000000000000000   00000010100000000000001010001000000   0000000100000000000000500000000   000000000000100000000000000000   000000000000010000000000000000   9009009009008908509001050890910890850910910910910910910910930100010508508501050未焙烧900900未焙烧1050
标有*的样品号不在本发明的范围之内
**CT：CaTiO3
***AL：Al2O3，Ti：TiO2，Zr：ZrO2，MT：MgTiO3，BT：BaTi4O9，LT：La2Ti2O7，NT：Nd2Ti2O7，
CN：Ca2Nb2O7，SZ：SrZrO3，CZ：CaZrO3
表2
序号   弯曲强度MPa   热膨胀系数×10-6/℃   9～15GHz下的特性 介电陶瓷中的晶相**
  εr   τf×10-6/℃   TCC×10-6/℃
  12345678*910111213141516171819202122*232425   251281274308270265263252276322299305318360264364360342326308263258240260280   8.58.58.58.58.48.58.58.58.49.39.49.59.38.99.39.38.99.298.99.39.59.79.69.2   10.010.89.410.08.89.312.515.98.110.19.89.69.59.48.79.09.19.49.38.712.9227.9813.4   18.822.7-16.6-2.2-35.1-21.759.359.0-63.33.9-1.1-2.1-12.3-9.9-31.4-25.9-26.3-18.2-14.3-165559.9-69.0-58.059   -54.6-62.416.2-12.5853.426.4-135.6-135109.8-26.4-16.6-14.86244.233.234.81810.614.2-128.6-138.8118.696.8-136.4   D，CT，H，AL，W，GD，CT，H，AL，W，GD，CT，H，AL，WD，CT，H，AL，WD，CT，H，AL，WD，CT，H，AL，WD，CT，ST，H，AL，WD，CT，ST，H，AL，W，N T，C ND，H，AL，WD，CT，AL，AD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，AL，NT，Co，SpD，CT，AL，NT，CN，MD，CTD，CT，ALD，CT，AL，NT
  *26   因未焙烧而未评估   -   -   -   -
  *27*28   340220   97   7.78.5   -67.75.5   117.4-25   D，ALCT，AL，Ce
  *29   因未焙烧而未评估   -   -   -   -
  *30   310   9.4   25   99.9   -218.6   D，CT，AL
标有*的样品号不在本发明的范围之内
**D：透辉石，H：锌黄长石，Ce：钡长石，Co：堇青石，G：锌尖晶石，
W：硅锌矿，Sp：尖晶石，M：富铝红柱石，CT：CaTiO3，ST：SrTiO3，
AL：Al2O3，CN：Ca2Nb2O7，NT：Nd2Ti2O7，A：钙长石
从表2的结果可以很明显地看出，样品号1～8、10～22、24和25中，任何介电陶瓷组合物都可以在850～1050℃的温度下，和诸如Ag或Cu的低电阻导体一起焙烧。
这些样品具有如下极好的介电特性：相对介电常数为8～22，陶瓷的三点弯曲强度为250MPa或更大，共振频率的温度系数为0±60×10-6/℃，静电容的温度系数为0±150×10-6/℃。特别是在介电陶瓷静电容的温度系数被控制在0±40×10-6/℃的样品中，静电容的温度系数为0±70×10-6/℃。
另一方面，在样品号9、23和26～30，这些不含钛酸钙或所含透辉石结晶玻璃粉和钛酸钙的数量不在本发明范围之内的样品中，三点弯曲强度小于250MPa，或者共振频率的温度系数不在0±60×10-6/℃范围内。
实施例2
采用与实施例1相同的方法，只是用平均颗粒大小为2μm的钛酸锶粉(纯度：99％或更高)取代实施例1中用作生粉的钛酸钙粉，制造并评估介电陶瓷。该组合物列于表3，评估结果见表4。
表3
  序号   玻璃    ST**(重量％)   填料组成(重量％)***   焙烧温度℃
组分 重量％ AL Ti Zr MT BT LT NT CN SZ CZ
  31323334353637383940414243444546474849*505152*53*54   AAAAAABBBBBBBBBBBBBBBBBB   606563726560607080726252746555535450459363303040   9562121399106775556620404220545   30293025117302092230402130394140200335406515   100000100000000000000000   011000010000000000000000   000100001000000000000000   000010000000000000000000   000010000000000000000000   00001010000000000001010001000   0000010000000000000500000   000000000010001000000000   000000000001000000000000   9009009008909001050910890850910910910910910910910910105010508508501050未焙烧1050
标有*的样品号不在本发明的范围之内
**ST：SrTiO3
***AL：Al2O3，Ti：TiO2，Zr：ZrO2，MT：MgTiO3，BT：BaTi4O9，LT：La2Ti2O7，NT：Nd2Ti2O7，
CN：Ca2Nb2O7，SZ：SrZrO3，CZ：CaZrO3
表4
序号   弯曲强度MPa   热膨胀系数×10-6/℃   9～15GHz下的特性 介电陶瓷中的晶相**
  εr   τf×10-6/℃   TCC×10-6/℃
  31323334353637383940414243444546474849*505152   250270305255250255312305305305302255255350350350350290270220255255   8.78.78.78.58.78.79.49.59.79.49.499.49.499.39.19.49.69.89.89.3   10.19.29.88.712.115.59.79.49.29.99.18.98.38.68.79.08.912.521.57.5813   53.613.823.8-16.155.059.053.653.659.923.833.733.713.813.813.823.823.85559.93.8-16.459.0   -124.6-45-6515.2-127.4-135.4-126-126.2-139.2-66.4-86.2-85.4-46.4-46.4-45.6-66.2-65.8-128.8-139-27.213.2-136.6   D，ST，H，AL，W，GD，ST，H，AL，WD，ST，H，AL，WD，ST，H，AL，WD，ST，H，AL，W，NT，CeD，ST，H，AL，W，NT，CND，ST，AL，AD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，CT，AL，NT，Co，SpD，CT，AL，NT，CN，MD，STD，ST，ALD，ST，AL，NT
  *53   因未焙烧而未评估   -   -   -   -
  *54   295   9.6   24.5   99.9   -219   D，ST，AL
标有*的样品号不在本发明的范围之内
**D：透辉石，H：锌黄长石，Ce：钡长石，Co：堇青石，G：锌尖晶石，
W：硅锌矿，Sp：尖晶石，M：富铝红柱石，CT：CaTiO3，ST：SrTiO3，AL：Al2O3，
CN：Ca2Nb2O7，NT：Nd2Ti2O7，A：钙长石
表4中的结果很清楚地表明，本发明的样品号31～49、51和52中，任何介电陶瓷组合物都可以在850～1050℃的温度下和诸如Ag或Cu的低电阻导体一起焙烧。
这些样品具有如下极好的介电特性：相对介电常数为8～21.5，陶瓷的三点弯曲强度为250MPa或更大，共振频率的温度系数为-16.4×10-6/℃～59.9×10-6/℃，静电容的温度系数为-139.2×10-6/℃～15.2×10-6/℃。
另一方面，在样品号50、53和54这些所含透辉石结晶玻璃粉和钛酸锶的数量不在本发明范围之内的样品中，无法进行烧结，或者其三点弯曲强度小于250MPa，或共振频率的温度系数不在0±60×10-6/℃范围内。
实施例3
采用与实施例1相同的方法，只是用平均颗粒大小分别为2μm、99％或更高纯度的钛酸钙粉和钛酸锶粉取代在实施例1中用作生粉的钛酸钙粉，制造并评估介电陶瓷。该组合物列于表5中，评估结果见表4。
表5
  序号   玻璃   CT**(重量％)   ST**(重量％)   填料组成(重量％)***   焙烧温度℃
组分 重量％ AL Ti Zr MT BT LT NT CN SZ CZ
  55565758596061   BBBBBAA 58584848726055   3111744   462039111   3535212203540   0000000   0000000   0000000   0000000   0000000   0010101000   0000000   0000000   0000000   900900900930930930900
**CT：CaTiO3，ST：SrTiO3
***AL：Al2O3，Ti：TiO2，Zr：ZrO2，MT：MgTiO3，BT：BaTi4O9，LT：La2Ti2O7，NT：Nd2Ti2O7，
CN：Ca2Nb2O7，SZ：SrZrO3，CZ：CaZrO3
表6
  序号   弯曲强度MPa   热膨胀系数×10-6/℃   9～15GHz下的特性   介电陶瓷中的晶相**
εr τf×10-6/℃ TCC×10-6/℃
  55565758596061   290277260260309268250   9.39.49.59.59.38.58.5   9.08.915.021.09.39.18.0   -29.9-39.9-50.0-59.0-16.5-16.9-20.9  41.261819914.416.824.8   D，CT，H，AL，STD，CT，H，AL，STD，CT，H，AL，ST，NTD，CT，H，AL，ST，NTD，CT，ST，ALD，CT，ST，H，AL，WD，CT，ST，H，AL，W
**D：透辉石，H：锌黄长石，W：硅锌矿，ST：SrTiO3，AL：Al2O3，
NT：Nd2Ti2O7
表6的结果很清楚地表明，本发明的样品号55～61中，任何介电陶瓷组合物都可以在900～930℃的温度下和诸如Ag或Cu的低电阻导体一起焙烧。
这些样品具有如下极好的介电特性：相对介电常数为8～21，陶瓷的三点弯曲强度为250MPa或更大，共振频率的温度系数为-59×10-6/℃～16.5×10-6/℃，静电容的温度系数为14.4×10-6/℃～99×10-6/℃。特别是在介电陶瓷静电容的温度系数被控制在0±40×10-6/℃的样品中，静电容的温度系数为0±70×10-6/℃。
实施例4
首先，称重玻璃料，该玻璃料是能够沉积透辉石晶体的结晶玻璃粉，CaTiO3，SrTiO3及Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3粉，每种粉的纯度为99％或更高，以及Fe2O3，Cr2O3，ZnO，CuO，Ag2O，Co3O4，MnO2，CeO2和R2O3(R代表稀土元素)，并将玻璃料按表7～9所示的比例和水混合，在使用ZrO2球的球磨机中湿化处理(介质：异丙醇)20小时，得到颗粒大小为2.0μm或更小的磨碎的混合物。
使用如下的玻璃料。
玻璃料D：41重量％SiO2-23重量％CaO-15重量％MgO-21重量％ZnO
玻璃料E：49重量％SiO2-33重量％CaO-18重量％MgO
样品号89中，使用玻璃料C作为比较例。用所得的混合物制造介电陶瓷，并用与实施例1相同的方法进行评估。目测介电陶瓷的褪色现象和色调。结果见表10～12。
表7
  序号   玻璃 CT**(重量％)   填料组成(重量％)***   添加剂组成(重量份数) 焙烧温度℃
组分 重量％ AL Ti Zr MT BT LT NT CN SZ CZ   Fe2O3   Cr2O3   ZnO   CuO   Ag2O   Co3O4   MnO2   CeO2    R2O3(R表示稀土元素)
  Y2O3   La2O3   Nd2O3   Sm2O3   Er2O3
  6263646566676869*7071727374757677787980818283*848586*87*88*89*90*91   DDDDDDDDDEEEEEEEEEEEEEEEEEECEE   607065687275656060607080625274645458534850459590302070603040   10105735131509910686667772040522040010545   291929242420105403020929392030403540452000640403030655   110000000101000000000000000000   001100000000100000000000000000   000010000001000000000000000000   000000100000000000000000000000   000000100000000000000000000000   00000010100000000000001010001000000   0000000100000000000000500000000   000000000000100000000000000000   000000000000010000000000000000   0.10.10.10.10.20.20.10.10.10.10.10.10.10.10.10.10.10.10.511.522.20.10.10.1010.10.05   00.10.10000.510000000000000000000100   000.1000001000000000000000000100   0000.100000100000000000000000000   000000000010000000000000000000   000000000001000000000000000000   000000000000000000000000000000   000000000000100000000000000000   000000000000010000000000000000   000000000000001000000000000000   000000000000000100000000000000   000000000000000010000000000000   000000000000000001000000000000   9009009009008908509001050890910890850910910910910910910910930100010508508501050未焙900900未焙1050
标有*的样品号不在本发明的范围之内
**CT：CaTiO3
***AL：Al2O3，Ti：TiO2，Zr：ZrO2，MT：MgTiO3，BT：BaTi4O9，LT：La2Ti2O7，NT：Nd2ALTi2O7，CN：Ca2Nb2O7，SZ：SrZrO3，CZ：CaZrO3
表8
序号   玻璃 ST**(重量％)   填料组成(重量％)***   添加剂组成(重量份) 焙烧温度℃
组分 重量％ AL Ti Zr MT BT LT NT CN SZ CZ Fe2O3 Cr2O3 ZnO CuO Ag2O Co3O4 MnO2 CeO2    R2O3(R表示稀土元素)
Y2O3 La2O3 Nd2O3 Sm2O3 Er2O3
  929394959697*9899100101102103104105106107108109110111*112113114*115*116   DDDDDDDEEEEEEEEEEEEEEEEEE   60656372656060607080726252746555535450459363303040   95621213099106775556620404220545   30302925117403020921304021304036402000940655   1000000100000000000000000   0110000010000000000000000   0001000001000000000000000   0000100000000000000000000   0000100000000000000000000   000010100000000000001010001000   00000100000000000000500000   0000000000010001000000000   0000000000001000000000000   0.10.10.10.20.10.10.10.10.10.10.10.10.10.10.10.10.10.51.522.20.10.10.10.05   00.1000.510000000000000000000   00.100001000000000000000000   000.10000100000000000000000   0000000010000000000000000   0000000001000100000000000   0000000000100010000000000   0000000000010000000000000   0000000000001000000000000   0000000000000100000000000   0000000000000010000000000  0000000000000001000000000   0000000000000000100000000 9009009008909001050890910890850910910910910910910910910105010508508501050未焙烧1050
标有*的样品号不在本发明的范围之内
**ST：SrTiO3
***AL：Al2O3，Ti：TiO2，Zr：ZrO2，MT：MgTiO3，BT：BaTi4O9，LT：La2Ti2O7，NT：Nd2Ti2O7，CN：Ca2Nb2O7，SZ：SrZrO3，CZ：CaZrO3
表9
序号   玻璃 CT**(重量％) ST**(重量％)   填料组成(重量％)***   添加剂组成(重量份) 焙烧温度℃
组分 重量％ AL Ti Zr MT BT LT NT CN SZ CZ Fe2O3 Cr2O3 ZnO CuO Ag2O Co3O4 MnO2 CeO2    R2O3(R表示稀土元素)
  Y2O3   La2O3   Nd2O3   Sm2O3   Er2O3
117118119120121122123124 EEEEEEDD 5858584848726055 53111744 2462039111 353535212203540 00000000 00000000 00000000 00000000 00000000 00010101000 00000000 00000000 00000000 0.10.10.10.10.10.10.10.1 0000000.10.2 00000000 00000000 0000000.10 00000000 00000000 00000000 00000000 00000000 00000000 00000000 000.50.50.50.500 900900900930930930900900
**CT：CaTiO3，ST：SrTiO3
***AL：Al2O3，Ti：TiO2，Zr：ZrO2，MT：MgTiO3，BT：BaTi4O9，LT：La2Ti2O7，NT：Nd2Ti2O7，CN：Ca2Nb2O7，SZ：SrZrO3，CZ：CaZrO3
表10
序号   弯曲强度MPa   热膨胀系数×10-6/℃   9～15GHz下的特性 着色或者防止褪色 色调 介电陶瓷中的晶相**
  εr   τf×10-6/℃   TCC×10-6/℃
  6263646566676869*7071727374757677787980818283*848586   251281274308270265263252276322299305318360264364360342326308263258240260280   8.58.58.58.58.48.58.58.58.49.39.49.59.38.99.39.38.99.298.99.39.59.79.69.2   9.810.69.29.88.69.112.315.77.99.99.79.49.39.28.58.88.99.29.18.512.721.87.77.813.2   18.822.7-16.6-2.2-35.1-21.759.359.0-63.33.9-1.1-2.1-12.3-9.9-31.4-25.9-26.3-18.2-14.3-165559.9-69.0-58.059   -54.6-62.416.2-12.5853.426.4-135.6-135109.8-26.4-16.6-14.86244.233.234.81810.614.2-128.6-138.8118.696.8-136.4   是是是是是是是是是是是是是是是是是是是是是是是是是   红棕棕棕红红棕棕棕棕棕棕棕红红红红红红红红红红红红   D，CT，H，AL，W，GD，CT，H，AL，W，GD，CT，H，AL，WD，CT，H，AL，WD，CT，H，AL，WD，CT，H，AL，WD，CT，ST，H，AL，WD，CT，ST，H，AL，W，N T，CND，H，AL，WD，CT，AL，AD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，ALD，CT，AL，NT，Co，SpD，CT，AL，NT，CN，MD，CTD，CT，ALD，CT，AL，NT
*87   因未焙烧而未评估   -   -   -   是   红   -
  *88*89   340220   97   7.78.3   -67.75.5   117.4-25   否是   白棕   D，ALCT，AL，C e
*90   因未焙烧而未评估 - - - 是 红 -
  *91   310   9.4   24.8   99.9   -218.6   否   白   D，CT，AL
标有*的样品号不在本发明的范围之内
**D：透辉石，H：锌黄长石，Ce：钡长石，Co：堇青石，G：锌尖晶石，
w：硅锌矿，Sp：尖晶石，M：富铝红柱石，
CT：CaTiO3，ST：SrTiO3，AL：Al2O3，CN：Ca2Nb2O7，
NT：Nd2Ti2O7，A：钙长石
表11
序号   弯曲强度MPa  热膨胀系数×10-6/℃   9～15GHz下的特性 着色或者防止褪色 色调 介电陶瓷中的晶相**
  εr   τf×10-6/℃   TCC×10-6/℃
  9293949596979899100101102103104105106107108109110111*112113114   250270305255250255270312305305305302255255350350350350290270220255255  8.78.78.78.58.78.78.59.49.59.79.49.499.49.499.39.19.49.69.89.89.3   9.99.09.68.511.915.37.89.59.29.09.78.98.78.18.48.58.88.712.321.37.37.412.8   53.613.823.8-16.155.059.0-36.053.653.659.923.833.733.713.813.813.823.823.85559.93.8-16.459.0   -124.6-45-6515.2-127.4-135.455-126-126.2-139.2-66.4-86.2-85.4-46.4-46.4-45.6-66.2-65.8-128.8-139-27.213.2-136.6   是是是是是是是是是是是是是是是是是是是是是是是   棕棕棕红棕棕棕棕棕棕棕棕红红红红红红红红红红红   D，ST，H，AL，W，GD，ST，H，AL，WD，ST，H，AL，WD，ST，H，AL，WD，ST，H，AL，W，NT，CeD，ST，H，AL，W，NT，CND，H，AL，WD，ST，AL，AD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，ST，ALD，CT，AL，NT，Co，SpD，CT，AL，NT，CN，MD，STD，ST，ALD，ST，AL，NT
*115   因未焙烧而未评估   -   -   -   是   -   -
  *116   295  9.6   24.3   99.9   -219   否   -   D，ST，AL
标有*的样品号不在本发明的范围之内
**D：透辉石，H：锌黄长石，Ce：钡长石，Co：堇青石，G：锌尖晶石，W：硅锌矿，Sp：尖晶石，
M：富铝红柱石，
CT：CaTiO3，ST：SrTiO3，AL：Al2O3，CN：Ca2Nb2O7，NT：Nd2Ti2O7，
A：钙长石
表12
序号   弯曲强度MPa   热膨胀系数×10-6/℃   9～15GHz下的特性 着色或者防止褪色   色调   介电陶瓷中的晶相**
  εr  τf×10-6/℃   TCC×10-6/℃
  117118119120121122123124   282290277260260309268250   9.29.39.49.59.59.38.58.5   8.88.88.714.820.89.18.97.8  -19.9-29.9-39.9-50.0-59.0-16.5-16.9-20.9   21.441.261819914.416.824.8   是是是是是是是是   红红红红红红棕棕   D，CT，H，AL，STD，CT，H，AL，STD，CT，H，AL，STD，CT，H，AL，ST，NTD，CT，H，AL，ST，NTD，CT，ST，ALD，CT，ST，H，AL，WD，CT，ST，H，AL，W
**D：透辉石，H：锌黄长石，W：硅锌矿，CT：CaTiO3，ST：SrTiO3，AL：Al2O3，
NT：Nd2Ti2O7
表10～12的结果很清楚地表明，本发明的样品号62～69，71～83，85，86，92～97，99～111，113，114和117～124中，这些样品使用钛酸钙、钛酸锶或钛酸钙和钛酸锶的混合物在介电陶瓷组合物中作为填料，任何介电陶瓷组合物都可以在850～1050℃的温度下和诸如Ag或Cu的低电阻导体一起焙烧。
无论进行着色与否，这些样品都具有如下极好的介电特性：相对介电常数为8～25，陶瓷的三点弯曲强度为250MPa或更大，共振频率的温度系数为0±60×10-6/℃，静电容的温度系数为0±150×10-6/℃。
另一方面，在样品号70，84，87～91，98，112，115和116这些透辉石结晶玻璃粉和填料组分的含量不在本发明范围之内的样品中，其三点弯曲强度小于250MPa，或其共振频率的温度系数τf不在0±60×10-6/℃范围内。

Claims (13)

1.一种介电陶瓷，其是通过焙烧介电陶瓷组合物而得到的，其中相对介电常数为8～22，陶瓷的三点弯曲强度为250MPa或更大，共振频率的温度系数为0±60×10-6/℃，所述的介电陶瓷组合物包含：
30～90重量％的能够沉积透辉石晶体的结晶玻璃粉，
1～40重量％的钛酸钙粉，钛酸锶粉或其混合粉末，以及
0～60重量％的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末。
2.权利要求1的介电陶瓷，其中所述的组合物包含30～90重量％的能够沉积透辉石晶体的结晶玻璃粉，1～40重量％的钛酸钙粉，以及0～60重量％的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末。
3.权利要求1的介电陶瓷，其中所述的组合物包含30～90重量％的能够沉积透辉石晶体的结晶玻璃粉，1～40重量％的钛酸锶粉，以及0～60重量％的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末。
4.权利要求1的介电陶瓷，其中所述的组合物包含30～90重量％的能够沉积透辉石晶体的结晶玻璃粉，总共1～40重量％的钛酸钙粉和钛酸锶粉，以及0～60重量％的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末。
5.权利要求1的介电陶瓷，其中能够沉积透辉石晶体的结晶玻璃粉、钛酸钙粉、钛酸锶粉或其混合粉的平均颗粒大小为3μm或更小。
6.权利要求1的介电陶瓷，其中静电容的温度系数为0±150×10-6/℃。
7.权利要求1的介电陶瓷，其中至少透辉石和/或透辉石固溶体和钛酸钙和/或钛酸锶是作为晶相共存的。
8.权利要求1的介电陶瓷，其中在室温～400℃下测得的热膨胀系数为8×10-6/℃或更高。
9.一种介电陶瓷组合物，该组合物包含：
100重量份的混合粉末，该混合粉末含30～90重量％的能够沉积透辉石晶体的结晶玻璃粉，1～40重量％的钛酸钙粉、钛酸锶粉或其混合粉，和0～60重量％的至少一种选自Al2O3，TiO2，ZrO2，MgTiO3，BaTi4O9，La2Ti2O7，Nd2Ti2O7，Ca2Nb2O7，SrZrO3和CaZrO3的粉末，以及
0.1～2.0重量份的至少一种选自Fe2O3，Cr2O3，ZnO，CuO，Ag2O，Co3O4，MnO2，CeO2和R2O3的粉末，其中R表示稀土元素。
10.在850～1050℃下焙烧含权利要求9的介电陶瓷组合物的混合物预成型坯而获得的介电陶瓷。
11.权利要求10的介电陶瓷，其中相对介电常数为8～22，陶瓷的三点弯曲强度为250MPa或更大，共振频率的温度系数为0±60×10-6/℃。
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