CN1065218C - 介电陶瓷组合物 - Google Patents

介电陶瓷组合物 Download PDF

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CN1065218C
CN1065218C CN96105570A CN96105570A CN1065218C CN 1065218 C CN1065218 C CN 1065218C CN 96105570 A CN96105570 A CN 96105570A CN 96105570 A CN96105570 A CN 96105570A CN 1065218 C CN1065218 C CN 1065218C
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佐佐木则夫
渡边义春
高桥幸治
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Abstract

具有由式(1)表示的组合物的介电陶瓷组合物；式(1)为：
(BaTiO3)e+(BaZrO3)f+(CaTiO3)g+(MgTiO3)h+(R1+R2+R3+R4) (1)
式中e为60.3-67.5mol%，f为11.9-15.6mol%，g为15.8-23.0mol%，和h为2.6-5.8mol%，只要e，f，g，和h的总量为100mol%；和R1为0.05-0.4Wt%NiO，R2为0.05-0.3Wt%CeO2，R3为0.03-0.2Wt% MnO，和 R4为0.0-0.25wt% SiO2，全部按BaTiO3，BaZrO3，CaTiO3和MgTiO3的总量100mol%计。

Description

介电陶瓷组合物
本发明涉及介电陶瓷组合物，尤其涉及高介电常数介电陶瓷组合物，它们适用于具有介电常数为4000或更高和高击穿电压的高电压电容器。
以BaTiO3-BaZrO3-CaTiO3-MgTiO3体系的陶瓷组合物用作主要组分的高介电常数介电陶瓷组合物(JP-A-3-65557和JP-A-3-65558)广泛地被用作陶瓷电容器，多层电容器，高频电容器，高压电容器等。(本文中的术语“JP-A”是指未经审查公开的日本专利申请。)
但是，由于这类传统的BaTiO3-BaZrO3-CaTiO3-MgTiO3体系的介电陶瓷组合物是铁电的，因此当相对介电常数为4000或更高时，难以通过降低介电损耗以确保4KV／mm或更高的高交变击穿电压。
鉴于以上情况，因此，本发明的目的是提供一种高介电常数介电陶瓷组合物，该组合物的相对介电常数为4000或更高，高交变击穿电压为4KV／mm或更高和很小的介电损耗。
本发明的其它目的和作用从下面的描述将变得明显。
本发明涉及具有由式(1)表示组合物的介电陶瓷组合物，式(1)为：(BaTiO3)e+(BaZrO3)f+(CaTiO3)g+(MgTiO3)h+(R1+R2+R3+R4)  (1)
式中e为60．3-67．5mol％，f为11．9-15．6mol％，g为15．8-23．0mol％，和h为2．6-5．8mol％，只要e，f，g和h的总量为100mol％；和
R1为0．05-0．4wt％ NiO，R2为0．05-0．3wt％CeO2，R3为0．03-0．2wt％ MnO，和R4为0．0-0．25wt％ SiO2，全部按BaTiO3，BaZrO3CaTiO3和MgTiO3的总量100mol％计。
通过使用上述组合物，可获得高相对介电常数为4000或更高，高交变击穿电压为4KV／mm或更高，介电损耗小以及烧结程度极好的介电陶瓷组合物。
由BaTiO3，BaZrO3，CaTiO3和MgTiO3组成的组合物有时称为主要组分，而NiO，CeO2，MnO，和SiO2有时称为添加剂。
下面通过参照优选的实施方案(实施例)详细描述本发明，但不能将其看作是对本发明的限制。
现描述实施例的介电陶瓷组合物的生产步骤。
作为起始物料，以烧结后的组合物为表1和2所示的相应组分的相应量称量碳酸钡(BaCO3)，二氧化钛(TiO2)，氧化锆(ZrO2)，碳酸钙(CaCO3)，碳酸镁(MgCO3)，氧化镍(NiO)，二氧化铈(CeO2)，氧化锰(MnO)和二氧化硅(SiO2)，将由此制备的每一种原料混合物采用球磨机湿混16小时，脱水并干燥，然后在1160-1200℃下煅烧以引起化学反应。
在粗碎之后，采用球磨机进行细粉碎，脱水并干燥，然后与作为有机粘结剂的聚乙烯醇(PVA)混合，将获得的混合物进行造粒，尺寸选择，可获得粗粉末。将该粗粉末在300MPa的压力下模压，获得直径为16．5mm，厚为1．1mm的圆片状模压的产品。
将该模压的产品在1280-1340℃下的空气中烧结，可获得陶瓷材料。在由此获得的陶瓷材料的两侧施加银(Ag)浆，形成随后通过焊接在其上固定铅线而获得陶瓷电容器的印刷电极。然后，测量由此获得的每一件试样的电特性，结果示于表1和2中。
在测量表l和2中所示的各种电特性中，在频率为1KHz和电压为1V时测量相对介电常数(εs)和介电损耗(tanδ)，通过施加500V的直流电压测量绝缘电阻(IR)，击穿电压被定义为单位厚度的交变击穿电压(AC．Eb)，以及采用已经1320℃烧结的各试样检测烧结程度并定极好(⊙)，良好(○)和差(×)的等级进行评价。测量85℃时电容的变化率(△C)。系列○指本发明的试样，系列×指对比试样。
表1
  试样序号 范围     主要组分(mol％)     添加剂(wt％)   CsA1  canδA2(％) IR(Ω)A3×1011 AC·EbA4(KV/mm) △C(％)A5OS℃ 烧结
DaTiO3  DaZrO3  CaTiO3  MgTiO3  NiO CaO2  MnO SiO2
    1    ×     50.4     12.5     26.3     2.0  0.20  0.10  0.05  0.00  2610  0.90     5.7     3.1     -44    ○
    2    ○     63.2     12.2     21.6     3.0  0.20  0.10  0.05  0.00  4612  0.72     6.0     4.0     -49    ○
    3    ○     64.5     12.6     19.9     3.0  0.20  0.10  0.05  0.00  4929  0.74     6.0     4.7     -50    ○
    4    ○     66.0     12.0     10.1     3.1  0.20  0.10  0.05  0.00  5240  0.75     6.0     4.6     -53    ○
    5    ○     67.5     13.0     16.3     3.2  0.20  0.10  0.05  0.00  5674  0.76     4.0     4.2     -55    ○
    6    ○     66.0     13.9     16.1     3.2  0.20  0.10  0.05  0.00  5200  0.56     5.0     4.3     -53    ○
    7    ×     67.4     13.9     14.0     4.7  0.20  0.10  0.05  0.00  4370  0.40     3.3     2.5     -57    ○
    8    ○     66.1     14.0     16.0     3.1  0.20  0.10  0.05  0.00  4940  0.45     6.0     4.4     -54    ○
9 ○ 65.5     15.6     15.0     3.1  0.20  0.10  0.05  0.00  4620  0.31     6.3     4.6     -54    ○
    10    ×     69.2     10.6     17.2     3.0  0.20  0.10  0.05  0.00  5930  1.90     5.1     2.7     -41    ×
    11    ×     67.5     9.6     19.0     3.1  0.20  0.10  0.05  0.00  4050  2.70     7.1     2.7     -39    ×
    12    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.05  0.00  4409  0.01     6.5     4.0     -53    ○
    13    ○     63.9     13.4     20.1     2.6  0.20  0.10  0.05  0.00  4603  0.02     5.0     4.6     -55    ○
    14    ○     64.6     14.5     17.0     3.1  0.20  0.10  0.05  0.00  4626  0.76     7.0     4.6     -54    ○
    15    ×     63.0     14.0     19.3     2.1  0.20  0.10  0.05  0.00  4330  0.70     9.5     2.0     -50    ○
16 × 62.5 17.6 17.0 2.1 0.20 0.10 0.05 0.00 3450 0.64 0.0 4.6 -60 ×
    17    ○     60.3     12.0     23.0     3.9  0.20  0.10  0.05  0.00  4090  0.71     5.0     5.0     -50    ○
    18    ○     62.6     12.1     21.4     3.9  0.20  0.10  0.05  0.00  4634  0.61     3.3     4.5     -50    ○
    19    ○     61.9     12.0     21.2     4.9  0.20  0.10  0.05  0.00  4240  0.53     4.2     4.5     -49    ○
    20    ○     61.3     11.9     21.0     5.0  0.20  0.10  0.05  0.00  4176  0.71     4.1     4.7     -47    ○
    21    ×     65.6     12.5     15.6     6.3  0.20  0.10  0.05  0.00  3220  0.91     6.0     4.1     -51    ×
*1．介电常数；*2．介电损耗；*3．绝缘电阻；*4．击穿电压；*5．电容的变化率；*6．烧结程度
表2
试样序号 范围     主要组分(mol％)     添加剂(wt％)   CsA1  canδA2(％) IR(Ω)A3×1011  AC·EbA4(KV/mm) △C(％)A5OS℃ 烧结*6
DaTiO3 DaZrO3 CaTiO3 MgTiO3  NiO  CoO2  MnO  SiO2
    22    ○     62.5     13.1     21.4     3.0  0.05  0.10  0.05  0.00  4310  0.21     1.0     4.4     -45     ○
    23    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.05  0.00  4409  0.01     6.5     4.8     -53     ○
    24    ○     62.5     13.1     21.4     3.0  0.40  0.10  0.05  0.00  4250  0.70     6.3     4.9     -50     ○
    25    ×     62.5     13.1     21.4     3.0  0.50  0.10  0.05  0.00  3230  1.30     5.3     4.7     -47     ×
    26    ○     62.5     13.1     21.4     3.0  0.20  0.05  0.05  0.00  4310  0.40     5.7     4.7     -52     ◎
    27    ○     62.5     13.1     21.4     3.0  0.20  0.30  0.05  0.00  4160  0.30     9.5     5.3     -54     ○
    28    ×     62.5     13.1     21.4     3.0  0.20  0.35  0.05  0.00  3050  0.21     10.2     5.0     -50     ×
    29    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.03  0.00  4392  0.33     6.5     4.0     -51     ○
    30    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.10  0.00  4720  0.42     4.2     4.6     -53     ◎
    31    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.20  0.00  4170  0.35     4.7     4.6     -52     ○
    32    ×     62.5     13.1     21.4     3.0  0.20  0.10  0.50  0.00  2090  1.00     4.3     2.0     -50     ×
    33    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.05  0.05  4520  0.32     6.3     4.0     -50     ◎
    34    ○     62.5     13.1     21.4     3.0  0.20  0.10  0.05  0.25  4220  0.37     7.0     4.5     -46     ○
    35    ×     62.5     13.1     21.4     3.0  0.20  0.10  0.05  0.50  2930  0.40     7.1     3.5     -41     ×
    36    ×     62.5     13.1     21.4     3.0  0.00  0.00  0.00  0.00  1630  0.71     0.7     2.2     -32     ×
    37    ×     62.5     13.1     21.4     3.0  0.00  0.10  0.05  0.00  2730  0 36     0.9     2.9     -44     ×
    38    ×     62.5     13.1     21.4     3.0  0.20  0.00  0.05  0.00  3940  0.53     1.2     3.5     -47     ×
    39    ×     62.5     13.1     21.4     3.0  0.20  0.10  0.00  0.00  3210  0.60     1.2     4.5     -49     ×
*1．介电常数；*2．介电损耗；*3．绝缘电阻；*4．击穿电压；*5．电容的变化率；*6．烧结程度
在表1和2所示的介电陶瓷组合物的试样中，试样序号2-6，8，9，12-14，17-20，22-24，26，27，29-31，33和34，落在本发明介电陶瓷组合物的范围内，显示出极好的电特性，相对介电常数为4000或以上和交变击穿电压为4KV／mm或以上(优选地为4．5KV／mm或以上)。其烧结程度也比较好，试样序号26，30和33的介电陶瓷组合物尤其显示出极好的烧结程度。
另一方面，试样序号1，16，21，25，28，32和35-39的介电陶瓷组合物具有的相对介电常数低于4000，因此落在本发明的范围之外，试样序号1，7，10，11，15，32和35-38的介电陶瓷组合物因其低于4．0KV／mm的低交变击穿电压，所以也落在本发明的范围之外。此外，试样序号10，11，16，21，25，28，32和35-39的介电陶瓷组合物显示出差的烧结程度。
其次，下文描述限制本发明范围的原因。(1)作为主要组分的钛酸钡(BaTiO3)的含量：
当作为主要组分的钛酸钡的含量低于60．3mol％(试样序号1)时，相对介电常数急剧下降，并且交变击穿电压也下降。另一方面，当钛酸钡的含量大于67．5mol％(试样序号10)时，介电损耗急剧增加，而交变击穿电压下降。因此，要求钛酸钡的含量落在60．3-67．5mol％的范围内，优选地为60．3-66．0mol％，更优选地为62．0-63．0mol％。(2)作为主要组分的锆酸钡(BaZrO3)的含量：
当作为主要组分的锆酸钡的含量低于11．9mol％(试样序号10和11)时，介电损耗急剧增加，而交变击穿电压降低。另一方面，当锆酸钡的含量大于15．6mol％(试样序号16)时，介电损耗降低，但相对介电常数降低且由于温度电容的变化率变大。因此，要求锆酸钡的含量落在11．9-15．6mol％的范围内，优选地为12．1-15．6mol％更优选地为12．5-13．5mol％。(3)作为主要组分的钛酸钙(CaTiO3)的含量：
当作为主要组分的钛酸钙的含量低于15．8mol％(试样序号7)时，交变击穿电压急剧下降，而由于温度电容的变化率变大。另一方面，当钛酸钙的含量大于23．0mol％(试样序号1)时，相对介电常数急剧降低，交变击穿电压也降低。因此，要求钛酸钙的含量落在15．8-23．0mol％的范围内，优选地为20．5-22．0mol％。(4)作为主要组分的钛酸镁(MgTiO3)的含量：
当作为主要组分的钛酸镁的含量低于2．6mol％(试样序号15)时，交变击穿电压降低，而由于温度电容的变化率变大。另一方面，当钛酸镁的含量大于5．8mol％(试样序号21)时，相对介电常数降低，并且烧结程度变差。因此，要求钛酸镁的含量落在2．6-5．8mol％的范围内，优选地为2．6-3．9mol％，更优选地为2．5-3．5mol％。(5)作为添加剂的氧化镍(NiO)的含量：
当作为添加剂的氧化镍的含量低于0．05wt％(试样序号37)时，相对介电常数和交变击穿电压降低。另一方面，当氧化镍的含量大于0．4wt％(试样序号25)时，不仅相对介电常数降低和介电损耗增加，而且烧结程序变差。因此，要求氧化镍的含量落在0．05-0．4wt％的范围内，优选地为0．05-0．3wt％，更优选地为0．15-0．25wt％。(6)作为添加剂的二氧化铈(CeO2)的含量：
当作为添加剂的二氧化铈的含量低于0．05wt％(试样序号38)时，相对介电常数降低而介电损耗增加。另一方面，当二氧化铈的含量大于0．3wt％(试样序号28)时，不仅相对介电常数降低。由于温度电容的变化率变大，而且烧结程度变差。因此，要求二氧化铈的含量落在0．05-0．3wt％的范围内，优选地为0．05-0．18wt％，更优选地为0．10-0．18wt％。(7)作为添加剂的氧化锰(MnO)的含量：
当作为添加剂的氧化锰的含量低于0．03wt％(试样序号39)时，相对介电常数降低而烧结程度变差。另一方面，当氧化锰的含量大于0．2wt(试样序号32)时，相对介电常数和交变击穿电压急剧降低，介电损耗增加。因此，要求氧化锰的含量落在0．03-0．2wt％的范围内，优选地为0．03-0．05wt％。(8)作为添加剂的二氧化硅(SiO2)的含量：
当作为添加剂的二氧化硅的含量大于0．25wt％(试样序号35)时，相对介电常数急剧降低，交变击穿电压也降低。在这种情况下，由于在烧结时碱性原料粘附，所以烧结程度也变差。因此，要求二氧化硅的含量落在0．0-0．25wt％的范围内，优选地为0．0-0．05wt％，更优选地为0．0-0．01wt％。(9)添加剂的存在：
当完全没有上述添加剂(试样序号36)时，相对介电常数和交变击穿电压降低，烧结程度变差。
本发明介电陶瓷组合物具有的高相对介电常数为4000或更高，高交变击穿电压为4KV／mm或更高，介电损耗小并且由于温度电容变化率小。因此，尤其适于用作高电压电容器，高电压隔直流电容器等。
在参照具体的实施例详细地描述了本发明的同时，很显然，对于本技术领域的熟练技术人员来说，各种变化和改进都不违背本发明的精神和范围。

Claims (3)

1．具有由式(1)表示的组合物的介电陶瓷组合物，式(1)为：(BaTiO3)e+(BaZrO3)f+(CaTiO3)g+(MgTiO3)h+(R1+R2+R3+R4)    (1)
式中e为60．3-67．5mol％，f为11．9-15．6mol％，g为15．8-23．0mol％，和h为2．6-5．8mol％，只要e，f，g和h的总量为100mol％；和R1为0．05-0．4wt％ NiO，R2为0．05-0．3wt％ CeO2，R3为0．03-0．2wt％ MnO，和R4为0．0-0．25wt％ SiO2，全部接BaTiO3，BaZrO3，CaTiO3和MgTiO3的总量100mol％计。
2．按权利要求1中所请求保护的介电陶瓷组合物，其中e为60．3-66．0mol％，f为12．1-15．6mol％，g为15．8-23．0mol％，和h为2．6-3．9mol％，只要e，f，g和h的总量为100mol％；和
R1为0．05-0．3wt％ NiO，R2为0．05-0．18wt％ CeO2，R3为0．03-0．05wt％ MnO，和R4为0．0-0．05wt％ SiO2，全部按BaTiO3，BaZrO3，CaTiO3和MgTiO3的总量100mol％计。
3．按权利要求2中所请求保护的介电陶瓷组合物，其中e为62．0-63．0mol％，f为12．5-13．5mol％，g为20．5-22．0mol％，和h为2．6-3．5mol％，只要e，f，g，和h的总量为100mol％；和
R1为0．15-0．25wt％ NiO，R2为0．10-0．18wt％ CeO2，R3为0．03-0．05wt％ MnO，和R4为0．0-0．01wt％ SiO2，全部按BaTiO3，BaZrO3，CaTiO3和MgTiO3的总量100mol％计。
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