CN1173024A - 介电陶瓷组合物 - Google Patents

介电陶瓷组合物 Download PDF

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CN1173024A
CN1173024A CN97115584A CN97115584A CN1173024A CN 1173024 A CN1173024 A CN 1173024A CN 97115584 A CN97115584 A CN 97115584A CN 97115584 A CN97115584 A CN 97115584A CN 1173024 A CN1173024 A CN 1173024A
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dielectric ceramic
composition
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mno
ceramic compositions
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CN1090372C (zh
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南川忠洋
安藤阳
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Murata Manufacturing Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1254—Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R4/00—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation
    • H01R4/02—Soldered or welded connections
    • H01R4/028—Soldered or welded connections comprising means for preventing flowing or wicking of solder or flux in parts not desired
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R43/00—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors
    • H01R43/02—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors for soldered or welded connections
    • H01R43/0256—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors for soldered or welded connections for soldering or welding connectors to a printed circuit board
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/306—Lead-in-hole components, e.g. affixing or retention before soldering, spacing means
    • H05K3/308—Adaptations of leads
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/34—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
    • H05K3/3447—Lead-in-hole components

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Insulating Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Ceramic Capacitors (AREA)

Abstract

本发明揭示了一种介电陶瓷组合物,主要含有通式为(Sr1－xKx)2(Na1－xBix)Nb5O15的主要组分,其中x约为0.1至0.35,并相对于主要组分含有以CrO2、MnO2、Fe2O3、CoO和NiO计,约0.02至2.0%(重量)的Cr、Mn、Fe、Co和Ni中的至少一种。该组合物既不含Pb,也不含BaTiO3,但具有与BaTiO3类介电材料类似的介电常数。该组合物的介电常数随温度的变化率小。该组合物适用于电容器。

Description

介电陶瓷组合物
本发明涉及一种介电陶瓷组合物。
一般来说，用于陶瓷电容器的介电材料是含有诸如Pb(Mg1/3Nb2/3)O3-PbTiO3(下文中简称为PMN-PT)或BaTiO3的各种材料。
然而，由于PMN-PT类介电材料在烘焙时会放出Pb蒸气，因此它们的配方必须能补偿Pb的损失。另外，它们经常与坩埚反应。另一方面，BaTiO3类材料一般需要高的烘焙温度(约1300℃左右)，由此增加了烘焙的成本。因此，需要既不含Pb，也不含BaTiO3的介电材料。
本发明的目的是提供一种适用于电容器的介电陶瓷组合物，它既不含Pb，也不含BaTiO3，具有与BaTiO3类介电材料类似的介电常数，其特征在于介电常数随温度的变化率小。
本发明的介电陶瓷组合物主要含有通式为(Sr1-xKx)2(Na1-xBix)Nb5O15(其中x约为0.1至0.35)的主要组分，并相对于主要组分含有约0.02至2.0％(重量)的Cr、Mn、Fe、Co和Ni中的至少一种(以CrO2、MnO2、Fe2O3、CoO和NiO计)。
本发明的具有上述组成的介电陶瓷组合物的居里点接近室温，该组合物的介电常数图的峰具有平缓的斜率。结果，在室温下该组合物的介电常数在2200至3600左右，该组合物随温度的变化率小。
下面参照实施例对本发明进行描述。
实施例
首先制备原料SrCO3、Bi2O3、Nb2O5、K2CO3、Na2CO3和MnO2。
根据表1中所示的x值和MnO2的比例称重并混合，得到主要含(Sr1-xKx)2(Na1-xBix)Nb5O15并含有MnO2添加剂的陶瓷组合物。在表1中，带有(*)的样品在本发明的范围之外。
                                                 表1
   样品编号   X值    MnO2添加量(wt.％)   ε   tanδ(％)     ρ(Ω·cm)(x1012)       电容量温度变化率(％) 电容量对直流电场的依赖程度(％)
  最大值    最小值
  *1   0     0.5  1100   12.0     0.8     +15     -3     5
  *2   0.05     0.5  1730   9.1     1.2     +14     -4     5
    3   0.10     0.5  2500   7.0     1.6     +13     -6     5
    4   0.15     0.5  3130   9.4     1.6     +24     -15     4
    5   0.20     0.5  3530   9.4     2.5     +12     -22     2
    6   0.225     0.5  3570   7.4     6.3     +3     -22     1
    7   0.25     0.5  3250   4.9     11.6     0     -20     0
    8   0.275     0.5  3010   4.0     10.0     0     -22     0
    9   0.30     0.5  2670   3.4     7.9     +1     -21     0
    10   0.35     0.5  2220   3.0     6.3     +1     -18     0
  *11   0.40     0.5  1770   3.1     6.0     +5     -16     0
    12   0.25     0.02  3060   9.0     9.8     +1     -20     0
    13   0.25     2.0  2380   5.5     8.5     +2     -22     1
  *14   0.25     2.5  1800   7.0     8.0     +1     -20     0
  *15   0.25     0.01                                      不烧结
  *16   0.25     无                                      不烧结
向每一种混合物中加入混合物重量的两倍的乙醇，然后在球磨机中湿研磨约5小时，干燥，在空气中700℃至900℃烘焙。
将该烘焙过的混合物进行粗研磨，然后与加入其中的预定量的有机粘合剂一起湿研磨5至10小时，脱水，然后通过40目筛分级。
然后将颗粒在750至1000kg/cm2压力下成型，得到直径为12mm，厚度为1.2mm的圆片，将这些圆片在空气中1100至1200℃下烘焙。由此得到各种介电陶瓷圆片。
将银电极糊料涂覆于各圆片的两表面形成银电极，并烘焙。由此得到各种陶瓷电容器圆片。
用下述方法测定这些陶瓷电容器圆片的电性能。
在20℃、1kHz频率和0.5V电压下测定各样品的电容量，相对于电极的面积和样品的厚度进行计算得到介电常数(ε)。在与测定介电常数的相同的条件下测定介电损耗(tanδ)。在20℃对各样品施加100V直流电压30秒，测定其电阻值，由此相对于样品的尺寸计算得到电阻率(ρ)。按以下所示得到各样品的电容量随温度变化的特性：在-25℃、0℃、+20℃、+40℃、+60℃和+85℃，1kHz的频率和0.5V交流电压下测定各样品的电容量，得到在所述各测定温度下相对于20℃电容量的电容量变化值，并得到随温度变化的最大值和最小值。按以下所示得到各样品的电容量对直流电场的依赖程度(表示各样品的电容量减小的程度)：将各样品置于1kV/mm直流电场中，测定在1kHz频率和0.5V交流电压下的电容量。根据在0V/mm直流电场中的电容量，从测得的值得到各样品的电容量对直流电场的依赖程度。
表1中列出了用上述方法测得的各样品的电性能数据，以及x值和加入MnO2的比例。
从这些数据中可以看出，本发明的样品的介电常数都在2220至3570范围内，与BaTiO3类介电材料的介电常数类似，而且这些样品的电容量对直流电场的依赖程度(表示各样品的电容量减小的程度)和电容量随温度的变化率较低。
下面说明对本发明的介电陶瓷组合物的组成范围进行限定的理由。
如果x小于约0.10(样品2)或者如果x高于约0.35(样品11)，则由于该组合物的介电常数低，且该组合物不具有与BaTiO3类介电材料类似的实用特性，所以是不适宜的。因此x的优选范围约为0.1至0.35，更好为约0.15-0.3。
对于添加剂MnO2，如果其量低于约0.02％(重量)(样品15)，则该陶瓷不能烧结；而如果该量高于约2.0％(重量)(样品14)，则该组合物的介电常数太低。因此，添加剂的量较好为0.02至2.0％(重量)，更好为约0.05-1.5。
在上述实施例中，MnO2用作添加剂。除了MnO2之外，也可将CrO2、Fe2O3、CoO、NiO和MnO2中的至少一种有效地加入本发明的组合物中，能得到同样的结果。
如上所述，本发明的介电陶瓷组合物虽然不含Pb，也不含Ba，仍然具有2200至3600左右的介电常数，这与BaTiO3类介电材料类似，而且该组合物的介电常数随温度的变化率令人满意地低。另外，该组合物还具有其它的优良特性。
因此，本发明的组合物适宜于用作介电材料，以提供小尺寸、大容量的陶瓷电容器(如叠层陶瓷电容器)。
虽然参照具体的实例对本发明进行了详细的叙述，但对本领域的技术人员来说，进行各种不脱离本发明的精神和范围的变化和修正将是显而易见的。

Claims (7)

1.一种介电陶瓷组合物，主要含有通式为(Sr1-xKx)2(Na1-xBix)Nb5O15的主要组分，其中x为0.10至0.35，并含有以CrO2、MnO2、Fe2O3、CoO和NiO计，占主要组分重量的0.02至2.0％的Cr、Mn、Fe、Co和Ni中的至少一种。
2.如权利要求1所述的介电陶瓷组合物，其特征在于x为0.15-0.3。
3.如权利要求2所述的介电陶瓷组合物，其特征在于含有以CrO2、MnO2、Fe2O3、CoO和NiO计，占主要组分重量的0.05至1.5％的Cr、Mn、Fe、Co和Ni中的至少一种。
4.如权利要求3所述的介电陶瓷组合物，其特征在于所述Cr、Mn、Fe、Co和Ni中的至少一种为Mn。
5.如权利要求1所述的介电陶瓷组合物，其特征在于含有以CrO2、MnO2、Fe2O3、CoO和NiO计，占主要组分重量的0.05-1.5％的Cr、Mn、Fe、Co和Ni中的至少一种。
6.如权利要求5所述的介电陶瓷组合物，其特征在于所述Cr、Mn、Fe、Co和Ni中的至少一种为Mn。
7.如权利要求1所述的介电陶瓷组合物，其特征在于所述Cr、Mn、Fe、Co和Ni中的至少一种为Mn。
CN97115584A 1996-07-26 1997-07-24 介电陶瓷组合物 Expired - Lifetime CN1090372C (zh)

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JP08197701A JP3087657B2 (ja) 1996-07-26 1996-07-26 誘電体磁器組成物
JP197701/96 1996-07-26

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EP0934595A2 (en) * 1997-05-30 1999-08-11 Phycomp Holding B.V. Ceramic multilayer capacitor and ceramic composition for use in such capacitor
JP2001506425A (ja) * 1997-10-08 2001-05-15 コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ セラミック多層キャパシタ
JP4396136B2 (ja) * 2003-05-21 2010-01-13 株式会社村田製作所 圧電磁器組成物およびそれを用いた圧電セラミック素子
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JP5087938B2 (ja) * 2007-02-01 2012-12-05 株式会社村田製作所 誘電体セラミック組成物及び積層セラミックコンデンサ
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JP3479324B2 (ja) * 1993-08-19 2003-12-15 日本特殊陶業株式会社 マイクロ波誘電体磁器組成物及びその製造方法
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CN1293573C (zh) * 2003-08-07 2007-01-03 松下电器产业株式会社 介电陶瓷组合物和采用其的陶瓷电子部件

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EP0820968A1 (en) 1998-01-28
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CN1090372C (zh) 2002-09-04
DE69701209T2 (de) 2000-09-28
EP0820968B1 (en) 2000-01-26
KR100207900B1 (en) 1999-07-15
TW373190B (en) 1999-11-01
DE69701209D1 (de) 2000-03-02
US5763346A (en) 1998-06-09
JPH1036172A (ja) 1998-02-10

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