CN1410390A - 介质陶瓷组成物以及使用它的电容器 - Google Patents

介质陶瓷组成物以及使用它的电容器 Download PDF

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CN1410390A
CN1410390A CN02143950A CN02143950A CN1410390A CN 1410390 A CN1410390 A CN 1410390A CN 02143950 A CN02143950 A CN 02143950A CN 02143950 A CN02143950 A CN 02143950A CN 1410390 A CN1410390 A CN 1410390A
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CN1216009C (zh
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的场弘明
佐野笃史
田村博
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Murata Manufacturing Co Ltd
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Abstract

一种介质陶瓷组成物以及使用它的电容器，由组成式为(Ba1－xCax)(Ti1－yZry)O3(其中：0＜x≤0.25，0＜y≤0.25)所表示的钛酸钡为主要成分的多晶固溶体所构成。相对于所述主要成分100重量部，将Y成分换算为Y2O3含有5重量部以下(其中：0重量部除外)，并且，将Mg成分换算为MgO含有2重量部以下(其中：0重量部除外)，将Al成分换算为Al2O3含有2.5重量部以下(其中：0重量部除外)。从而实现最大相对介电常数高、静电容量温度特性优异、且交流击穿电压高。

Description

介质陶瓷组成物以及使用它的电容器
技术领域
本发明是涉及一种介电常数高、静电容量温度特性平坦且交流击穿电压高的介质陶瓷组成物及其使用它的电容器。
背景技术
在被广泛用于单板陶瓷电容器、叠层陶瓷电容器、高频陶瓷电容器、以及高压陶瓷电容器等中的高介电常数磁性材料中，以BaO-CaO-TiO2-ZrO2系列的介质陶瓷组成物为主要成分的电容器已经实用化。
然而，现有的BaO-CaO-TiO2-ZrO2系列的介质陶瓷组成物，存在当相对介电常数变大时会产生静电容量温度特性变差，进而使交流击穿电压降低等问题。
作为解决这些问题的介质陶瓷组成物，在特开平7-267732号公告中虽然公开了一种方案，但在其实施例中的交流击穿电压最高也仅有4.5kV/mm。
发明内容
鉴于上述问题，本发明的目的在于，提供一种最大相对介电常数高、静电容量温度特性好且交流击穿电压高的介质陶瓷组成物及其使用它的电容器。
本发明之一中的介质陶瓷组成物具有以下特征：由组成式为(Ba1-xCax)(Ti1-yZry)O3(其中：0＜x≤0.25，0＜y≤0.25)所表示的钛酸钡为主要成分的多晶固溶体所构成。相对于所述主要成分100重量部，将Y成分换算为Y2O3含有5重量部以下(其中：0重量部除外)，并且，将Mg成分换算为MgO含有2重量部以下(其中：0重量部除外)，将Al成分换算为Al2O3含有2.5重量部以下(其中：0重量部除外)。
本发明之二中的介质陶瓷组成物具有以下特征：在对以所述钛酸钡为主要成分的多晶固溶体用组成式(Ba1-xCax)a(Ti1-yZry)bO3表示时，则0.965≤a/b≤1.03。
本发明之三中的介质陶瓷组成物具有以下特征：作为副成分，相对于主要成分100重量部，将Mn成分换算为MnO含有2重量部以下。
本发明之四中的介质陶瓷组成物具有以下特征：作为副成分，相对于主要成分100重量部，将Si成分换算为SiO2添加含有2重量部以下。
本发明之五中的介质陶瓷组成物具有以下特征：作为副成分，相对于主要成分100重量部，将Nb成分换算为Nb2O5含有1重量部以下。
本发明之六中的电容器具有以下特征：具有根据本发明之一所述的介质陶瓷组成物所组成的介质陶瓷板，和在该介质陶瓷板的两面形成的电极。
具体实施方式
下面用实施例对本发明的实施方式进行说明。
(实施例)
作为最初的原材料，准备碳酸钡(BaCO3)、碳酸钙(CaCO3)、二氧化钛(TiO2)、二氧化锆(ZrO2)、氧化铟(Y2O3)、氧化镁(MgO)、三氧化二铝(Al2O3)、氧化锰(MnO)、二氧化硅(SiO2)、五氧化二铌(Nb2O5)，并将这些原材料配合得到表1表2所示的最终值的组成物，球磨(ballmill)湿式混合后，蒸发干燥。
接着。将所得到的粉末混合物在1150℃预烧结2小时，得到所定化合物的粉末。
相对所得到的化合物粉末100重量部，添加5重量部的结合剂，即醋酸乙烯基(vinyl)系列粘结剂，球磨(ball mill)湿式混合。
将该混合物干燥，制粒得到粉末状，再以2.5t/cm3的压力，将该原料粉末成形为直径15mm，高度1.5mm的圆板状。
接着，将该圆板状成形体用电炉按照表1、表2中所示的温度在空气中烧结，得到陶瓷烧结体，在该陶瓷烧结体的两面涂附以银胶(paste)，在空气中800℃进行烧结，形成电极，再用锡焊的方法接续导线(lead)，得到作为试样的陶瓷电容器。
对由以上方法得到的试样，施加250V的电压2分钟，测量其绝缘电阻。
再在1kHz，1Vrms的条件下，测定其静电容量温度系数，以表示静电容量最大的温度为基准(0％)，算出距此±50℃的各温度下静电容量温度的变化率。使用这样的方法的理由如下。例如，在表示-25℃与+85℃的静电容量温度特性的场合，转移点就可能不是常温附近。如果以转移点的静电容量温度的变化率作为基准，来表示自转移点±50℃的各温度下静电容量温度的变化率，就能够容易地进行各试样的特性的比较。
最大相对介电常数(εmax)由下式算出。
    εmax＝(Cmax×T)/[ε0×(D/2)2×π]                (式1)
式中，Cmax：静电容量最大值(F)
      T：陶瓷的厚度(m)
      ε0：真空的介电常数(F/m)＝8.854×10-12
      D：陶瓷的直径(m)
      π：圆周率
另外，击穿电压是以厚度1mm的交流击穿电压而算出。
以上的结果表示在表1、表2中。该表中带有*的试样，不在本发明的范围。
这里对本发明中限制介质陶瓷组成物的成分范围的理由加以说明。
如试样序号10、11所示，Ca的含量超过0.25时，烧结性能低下，即使是在1400℃烧结，仍是烧结不充分。欲烧结好需要更高的温度，就会使生产成本上升，这是所不希望的。因此，希望Ca的含量为0＜x≤0.25。
如试样序号8、9所示，Zr的含量超过0.25时，烧结性能低下，即使是在1400℃烧结，仍是烧结不充分。欲烧结好需要更高的温度，就会使生产成本上升，这是所不希望的。因此，希望Ca的含量为0＜y≤0.25。
Y成分的添加，能够起到使静电容量温度特性平坦化的效果，如试样12所示，如果以Y2O3量为0重量部时转移点的静电容量温度变化率为基准，则自转移点±50℃下的静电容量温度的变化率超过了-60％，这是所不希望的。而且，如试样16所示，当Y2O3的量超过5时，εmax大幅度低下，小于6000，这也是所不希望的。因此，希望Y2O3的相对于主要成分的量在5以下(0的重量部除外)。
Mg成分的添加，能够起到使静电容量温度特性平坦化的效果，如试样17所示，如果以Mg氧的重量部为0时转移点的静电容量温度变化率为基准，则自转移点±50℃下的静电容量温度的变化率超过了-60％，这是所不希望的。而且，如试样20所示，当Y2O3的量超过2重量部时，εmax大幅度低下，小于6000，这也是所不希望的。因此，希望MgO的相对于主要成分的量在2重量部以下(0的重量部除外)。
Al成分的添加，能够起到使交流击穿电压增大的效果，如试样21所示，Al2O3的重量部为0时，交流击穿电压小于5.0Kv/mm，这是所不希望的。而且，如试样25所示，当Al2O3的量超过.52时，绝缘电阻小于1.0×1010，这也是所不希望的。因此，希望Al2O3的相对于主要成分的量在2.5重量部以下(0的重量部除外)。
这样，添加成分的Y2O3、MgO、Al2O3都是必须的。如果不能满足这一条件，如试样26-29所示，如果以转移点的静电容量温度变化率为基准，则自转移点±50℃下的静电容量温度的变化率超过了-60％，而且交流击穿电压也小于5.0kV/mm，这是所不希望的。
如试样31所示，当a/b小于0.965时，绝缘电阻小于1.0×1010，这是所不希望的，而且，当a/b大于1.03时，绝缘电阻小于1.0×1010，这也是所不希望的。因此，希望0.965≤a/b≤1.03。
Mn成分的添加，能够降低烧结温度，还能够起到使静电温度特性平坦化的效果。但是，当MnO的添加量超过2重量部时，如试样41所示，绝缘电阻小于1.0×1010，这也是所不希望的。因此，希望MnO的添加量相对于主成分在2以下。
Si成分的添加，能够起到降低烧结温度的效果。但是，当SiO2的添加量超过2重量部时，如试样46所示，绝缘电阻小于1.0×1010，这也是所不希望的。因此，希望SiO2的添加量相对于主成分在2重量部以下。
Nb成分的添加，能够起到降低烧结温度的效果。但是，当Nb2O5的添加量超过1重量部时，如试样51所示，绝缘电阻小于1.0×1010，这也是所不希望的。因此，希望Nb2O5的添加量相对于主成分在1重量部以下。
在本实施例中，作为出发原材料，将碳酸钡(BaCO3)、碳酸钙(CaCO3)、二氧化钛(TiO2)、二氧化锆(ZrO2)、氧化铟(Y2O3)、氧化镁(MgO)、三氧化二铝(Al2O3)、氧化锰(MnO)、二氧化硅(SiO2)、五氧化二铌(Nb2O5)按照目的组成物混合后，进行预烧结。但是，也可以预先将碳酸钡(BaCO3)、碳酸钙(CaCO3)、二氧化钛(TiO2)、二氧化锆(ZrO2)混合后预烧结，再添加氧化铟(Y2O3)、氧化镁(MgO)、三氧化二铝(Al2O3)、氧化锰(MnO)、二氧化硅(SiO2)、五氧化二铌(Nb2O5)等。
在本实施例中，是在磁件体的两侧形成电极而制作电容器。但是本发明也不限于该实施例，例如，可以由多个积层的介电体磁件层、该电体磁件层形成的内部电极、以及与该内部电极相接续的外部电极所构成，使用这样的多层电容器，可以得到同样的效果。
根据本发明，可以得到介电常数高至6000以上、静电容量温度特性优异，以转移点的静电容量温度特性为基准，自转移点±50℃的各温度下静电容量温度的变化率在-60％以内且平坦、交流击穿电压在5.0kV/mm以上的高介质陶瓷组成物。
而且，使用本发明的介质陶瓷组成物作为介质陶瓷，在其两面设置电极制作电容器，可以实现具有所述介质陶瓷组成物优异特性的陶瓷电容器。
表1
试样序号 a/b 主成分 添加成分 烧结温度(℃) 初期特性
Ba(1-x) Ca(x) Ti(1-y) Zr(y) Y2O3(重量部) MgO(重量部) Al2O3(重量部) MnO(重盐部) SiO2(重量部) Nb2O5(重量部) εmax 以表示静电容量为最大的温度为基淮(O%)i在距此-50℃时温度的容量温度变化率(％) 以表示静电容量为最大的温度为基准(0％)，在距此+50℃的温度的容量温度变化率(1％) 绝缘电阻(MΩ) 交流击穿电压(kV/mm)
1 1.003 0.950 0.050 0.860 0.140 1.0 0.2 0.2 0 0 0 1400 12500 -57 -56 8.6×1011  5.1
2 1.003 0.930 0.070 0.920 0.080 1.0 0.2 0.2 0 0 0 1.400 11600 -55 -54 7.1×1011 5.2
3 1.003 0.880 0.120 0.880 0.120 1.0 0.2 0.2 0 0 0 1400 10600 -54 -53 6.4×1011 5.3
4 1.003 0.860 0.140 0.820 0.180 1.0 0.2 0.2 0 0 0 1400 6200 -44 -45 7.8×1011 5.1
5 1.003 0.830 0.170 0.960 0.040 1.0 0.2 0.2 0 0 0 1400 6700 -48 -47 4.1×1011 5.2
6 1.003 0.B90 0.110 0.750 0.250 1.0 0.2 0.2 0 0 0 1400 8600 -49 -50 5.5×1011 5.4
7 1.003 0.750 0.250 0.880 0.120 1.0 0.2 0.2 0 0 0 1400 6400 -43 -48 3.9×1011 5.1
*8 1.003 0.960 0.040 0.700 0.300 1.0 0.2 0.2 0 0 0 1400                          烧结不充分
*9 1.003 0.860 0.140 0.700 0.300 1.0 0.2 0.2 0 0 0 1400                          烧结不充分
*10 1.003 0.700 0.300 0.840 0.160 1.0 0.2 0.2 0 0 0 1400                          烧结不充分
*11 1.003 0.700 0.300 0.930 0.070 1.0 0.2 0.2 0 0 0 1400                          烧结不充分
*12 1.001 0.930 0.070 0.920 0.080 0 0.4 0.3 0 0 0 1400 13900 -62 -67 2.0×1011 5.0
13 1.001 0.930 0.070 0.920 0.080 0.1 0.4 0.3 0 0 0 1.400 12100 -57 -58 3.4×1011 5.1
14 1.001 0.930 0.070 0.920 0.080 2.0 0.4 0.3 0 0 O 1400 9600 -54 -53 5.2×1011 5.2
15 1.001 O.930 0.070 0.920 0.080 5.0 0.4 0.3 0 0 0 1400 6300 -48 -45 7.9×1010 5.1
*16 1.001 0.930 0.070 0.920 0.080 6.0 0.4 0.3 0 0 0 1400 5800 -42 -44 8.1×109 5.1
*17 0.999 0.950 0.050 0.860 0.140 0.4 0 0.3 0 0 0 1390 12800 -61 -63 5.7×1011 5.0
18 0.999 0.950 0.050 0.860 0.140 0.4 0.1 0.3 0 0 0 1390 10500 -55 -56 6.1×1011 5.0
19 0.999 0.950 0.050 0.860 0.140 0.4 2.0 0.3 0 0 0 1400 8100 -51 -50 3.4×1011 5.1
*20 0.999 0.950 0.050 0.860 0.140 0.4 3.0 0.3 0 0 0 1400 5900 -43 -44 5.5×1011 5.1
*2f 1.007 0.870 0.130 0.800 0.200 1.2 0.3 0 0 0 0 1390 8400 -51 -51 1.4×1011 4.6
-22 1.007 0.870 0.130 0.800 0.200 1.2 0.3 0.1 0 0 0 1390 8200 -47 -49 3.1×1011 5.1
23 1.007 0.870 0.130 0.800 0.200 1.2 0.3 0.5 0 0 O 1390 8100 -48 -50 5.9×1011 5.4
24 1.007 0.870 0.130 0.800 0.200 1.2 0.3 2.5 0 0 0 1390 8200 -49 -51 6.3×1010 5.5
*25 1.007 0.870 0.130 0.800 0.200 1.2 0.3 5.0 0 0 0 1390 7800 -49 -48 5.4×108 5.2
*26 1.002 0.950 0.050 0.860 0.140 0 0 0 0 0 0 1400 15100 -76 -79 2.1×1011 4.5
*27 1.002 0.950 0.050 0.860 0.140 0.8 0 0 0 0 0 1400 14300 -68 -85 2.7×1011 4.6
*28 1.002 0.950 0.050 0.860 0.140 0 0.3 0 0 0 0 1400 13600 -65 -64 3.6×1011 4.7
*29 1.002 0.950 0.050 0.860 0.140 0 0 0.2 0 0 0 1400 15300 -77 -76 3.8×1011 5.1
30 1.002 0.950 0.050 0.860 0.140 0.8 0.3 0.2 0 0 0 1400 12900 -59 -57 4.9×1011 5.1
31 0.960 0.910 0.090 0.870 0.130 0.8 0.2 0.1 0 0 0 1390 12300 -82 -63 2.2×109 5.0
32 0.965 0.910 0.090 0.870 0.130 0.8 0.2 0.1 0 0 0 1390 12200 -59 -59 2.2×1011 5.1
33 0.985 0.910 0.090 0.870 0.130 0.8 0.2 0.1 0 0 0 1390 12100 -58 -57 3.4×1011 5.0
34 1.000 0.910 0.090 0.870 0.130 1.2 0.3 0.5 0 0 0 1390 11900 -56 -57 4.7×1011 5.2
35 1.030 0.910 0.090 0.870 0.130 0.8 0.2 0 0 0 0 1390 7000 -51 -49 6.8×1011 5.1
36 1.035 0.910 0.090 0.870 0.130 0.8 0.2 0.1 0 0 0 1390 5700 -46 -45 7.1×109 5.0
【表2】
 试样序号    a/b                     主成分                                     添加成分  烧结温度(℃)                                                         初期特性
   Ba(1-x)    Ca(K)     Ti(1-y)    Zr(v)     Y203(重量部)     MgO(重量部)     Al2O3(重量部)     MnO(重量部)    SiO2(重量部)   Nb2O5(重量部)   εmax 以表示静电容量为最大的温度为基准(0％)，在距此-50℃的温度的容量温度变化率(％)  以表示静电容量为最大的温度为基准(0％)，在距此+50℃的温度的容量温度变化率(％)  绝缘电阻(MΩ)   交流击穿电压(kV/mm)
    37   1.000   0.880   0.120   0.880   0.120     1.1     0.3     0.2     0     0     0   1390   10400      -55      -57  6.4×1011     5.2
    38   1.000   0.880   0.120   0.880   0.120     1.1     0.3     0.2     0.1     0     0   1380   9900      -53      -53  4.6×1011     5.1
    39   1.000   0.880   0.120   0.880   0.120     1.1     0.3     0.2     0.5     0     0   1370   8200      -47      -48  1.3×1011     5.2
    40   1.000   0.880   0.120   0.880   0.120     1.1     0.3     0.2     2.0     0     0   1360   6500      -43      -42  5.4×1010     5.0
    41   1.000   0.880   0.120   0.880   0.120     1.1     0.3     0.2     3.0     0     0   1360   5300      -40      -41  7.2×109     5.0
    42   1.007   0.870   0.130   0.800   0.200     2.0     0.2     0.1     0     0     0   1390   8300      -51      -52  5.1×1011     5.1
    43   1.007   O.870   0.130   0.800   0.200     2.0     0.2     0.1     0     0.2     0   1380   8100      -49      -50  4.4×1011     5.1
    44   1.007   0.870   0.130   0.800   O.200     2.0     0.2     0.1     0     0.5     0   1370   8300      -51      -49  6.7×1011     5.4
    45   1.007   0.870   0.130   0.800   0.200     2.0     0.2     0.1     0     2.0     0   1360   8200      -50      -48  1.4×1011     5.2
    46   1.007   0.870   0.130   0.800   0.200     Z.0     0.2     0.1     0     3.0     0   1360   8000      -49      -47  9.1×109     5.0
    47   1.006   0.950   0.050   0.B60   0.140     1.5     0.3     0.2     0     0     0   1380   11200      -56      -54  2.7×1011     5.2
    48   1.006   0.950   0.050   0.860   0.140     1.5     0.3     0.2     0     0     0.2   1380   11000      -55      -53  3.4×1011     5.1
    49   1.006   0.950   0.050   0.860   0.140     1.5     0.3     0.2     0     0     0.5   1380   10500      -54      -57  7.6×1011     5.3
    50   1.006   0.950   0.050   0.860   0.140     1.5     0.3     0.2     0     0     1.0   1380   10800      -53      -56  8.4×1011     5.2
    51   I.006   0.950   0.050   0.860   0.140     1.5     0.3     0.Z     0     0     2.0   1380   10300      -50      -54  6.4×109     5.0
    52   1.004   0.950   0.050   0.850   0.150     0.8     0.3     0.2     0     0.4     0.2   1380   11700      -54      -52  5.7×1011     5.0
    53   1.004   O.950   0.050   0.850   0.150     0.8     0.3     0.2     0.15     0     0.2   1380   11000      -53      -53  5.9×1011     5.7
    54   1.004   O.950   0.050   0.850   0.150     0.8     0.3     0.2     0.15     0.4     0   1370   10200      -49      -48  4.8×1011     5.4
    55   1.004   0.950   0.050   0.850   0.150     0.8     0.3     0.2     0.15     0.4     0.2   1370   10000      -50      -49  5.6×1011     5.3

Claims (6)

1.一种介质陶瓷组成物，其特征在于：由组成式为(Ba1-xCax)(Ti1-yZry)O3(其中：0＜x≤0.25，0＜y≤0.25)所表示的钛酸钡为主要成分的多晶固溶体所构成。相对于所述主要成分100重量部，将Y成分换算为Y2O3含有5重量部以下(其中：0重量部除外)，并且，将Mg成分换算为MgO含有2重量部以下(其中：0重量部除外)，将Al成分换算为Al2O3含有2.5重量部以下(其中：0重量部除外)。
2.根据权利要求1所述的介质陶瓷组成物，其特征在于：在对以所述钛酸钡为主要成分的多晶固溶体用组成式(Ba1-xCax)a(Ti1-yZry)bO3表示时，则0.965≤a/b≤1.03。
3.根据权利要求1或2所述的介质陶瓷组成物，其特征在于：作为副成分，相对于主要成分100重量部，将Mn成分换算为MnO含有2重量部以下。
4.根据权利要求1或2所述的介质陶瓷组成物，其特征在于：作为副成分，相对于主要成分100重量部，将Si成分换算为SiO2添加含有2重量部以下。
5.根据权利要求1或2所述的介质陶瓷组成物，其特征在于：作为副成分，相对于主要成分100重量部，将Nb成分换算为Nb2O5含有1重量部以下。
6.一种电容器，其特征在于：具有根据本发明之一所述的介质陶瓷组成物所组成的介质陶瓷板，和在该介质陶瓷板的两面形成的电极。
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