CN1374667A - 多层陶瓷电容及其生产方法 - Google Patents
多层陶瓷电容及其生产方法 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 5
- 239000000919 ceramic Substances 0.000 claims abstract description 53
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 7
- 239000011575 calcium Substances 0.000 claims description 28
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 17
- 229910052573 porcelain Inorganic materials 0.000 claims description 14
- 238000003475 lamination Methods 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000010953 base metal Substances 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910002971 CaTiO3 Inorganic materials 0.000 abstract 1
- 229910002976 CaZrO3 Inorganic materials 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 238000009413 insulation Methods 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
一种多层陶瓷电容器,其包括有包含主结晶相和次生相的烧结体。主结晶相主要包含CaTiO3和CaZrO3;次生相主要包含钙(Ca)、硅(Si)。次生相中的钙含有量等于或小于30mol%。
Description
技术领域
本发明涉及一种多层陶瓷电容的生产方法，特别是生产由CaTiO3/CaZrO3构成的多层陶瓷电容，这种多层陶瓷电容是在中性或还原气氛中烧制而成的。
背景技术
诸如多层陶瓷电容等陶瓷电子器件的内部电极多数由贱金属实现，如镍(Ni)、铜(Cu)，以减少材料成本；由于贱金属易被氧化，包含有贱金属内部电极的多层陶瓷电容所用的陶瓷需在中性或还原气氛中烧制。
在日本未审定专利申请63-126117中公开了一种介电陶瓷组合物，其能够在中性或还原气氛中烧制用于温度补偿。
此组合物的主要成分表示为(Ca1-xSrx)m(Zr1-yTiy)O3，这里变量x、y和m分别满足：0≤x≤0.6，0≤y≤0.6，0.85≤m≤1.30。另外，相对于重量一百份的主要成分，提供重量0.5-8份的MnO2和重量0.5-8份的包含TiO2、SiO2和类似成分的玻璃成分。
根据该专利公报，通过控制该介电陶瓷组合物的Ti/Zr比，能够大范围地控制多层陶瓷电容的温度特性。其温度特性表示温度与电容之间的一种变化率，通常称作温度系数，由ppm/℃表示。温度系数的定义可按下式得出：
温度系数＝(Ci-C0)×106/(Ti-T0)，这里Ci和C0分别是温度为Ti和T0时的电容值。
温度补偿陶瓷电容器的温度特性是由组合的两个字母字符表达的，一个代表温度系数，另一个代表温度系数的允许误差。按照该公报所述的介电陶瓷组合物实现了具有在CG和SL范围内的所希望的温度特性的多层陶瓷电容。
这里CG表示0ppm/℃的温度系数和±30ppm/℃的温度系数允许误差，SL表示在+350ppm/℃至-1000ppm/℃范围内的温度系数，如表1和表2所示。
表1
| 字符 | C | L | P | R | S | T | U | SL |
| 温度系数(ppm/℃) | 0 | -80 | -150 | -220 | -330 | -470 | -750 | -1000至+350 |
表2
| 字符 | K | J | H | G |
| 允差(ppm/℃) | ±250 | ±120 | ±60 | ±30 |
该公报还指出，提高钛(Ti)含量改善陶瓷电容的温度特性。
然而，由CaTiO3/CaZrO3生成的多层陶瓷电容，在高温负荷试验时可能会引起短路和绝缘电阻(IR)降低现象。
发明内容
本发明的目的在于提供一种可靠的多层CaTiO3/CaZrO3陶瓷电容器及其生产方法；这种陶瓷电容器在高温负荷试验中很少出现短路和绝缘电阻降低的情况，从而解决了前面所描述的问题。
为达到此目的，根据本发明的一个方面，提供了一种由烧结陶瓷体(sintered ceramic compact)组成的多层陶瓷电容，烧结陶瓷体包括主要包含有CaTiO3和CaZrO3的主结晶相(primary crystalline phase)和主要包含有钙(Ca)和硅(Si)的次生相(secondary phase)；在次生相中钙的含有量等于或少于30mol％。多层陶瓷电容还包括置于烧结陶瓷体中的内部电极。
为了降低多层陶瓷电容的材料成本，内部电极可以包括贱金属。
本发明的另外一个方面是提供一种生产多层陶瓷电容的方法。该方法包括步骤：制备一个绿瓷叠片(green ceramic laminate)，其包括：包括有CaTiO3和CaZrO3的主成分，包括有MnO2和SiO2的副成分，以及多个内部电极。该方法还包括步骤：在至少5℃/min的加热速率条件下，烧制绿瓷叠片至最高温度。
因此能够实现在高温负荷试验中具有高可靠性的多层陶瓷电容。
附图的简要说明
图1是本发明实施例的多层陶瓷电容器的截面图。
图2是说明图1所示的多层陶瓷电容主结晶相、次生相的截面图。
具体实施方案
本发明具体实施方案描述如下：
根据本发明多层陶瓷电容的烧结陶瓷体具有：主要包含CaTiO3和CaZrO3的主结晶相，和主要包含钙(Ca)和硅(Si)的次生相。这样的一种具有主结晶相和次生相的烧结陶瓷体，正如在日本未审定专利申请63-126117中所介绍的那样，是通过烧制相对于由通式(Ca1-xSrx)m(Zr1-yTiy)O3表示的100份重量的主要成分，重量为0.5-8份的MnO2和重量为0.5-8份的含TiO2、SiO2的玻璃成分制备的。
这里在该通式中的变量x、y和m分别满足：0≤x≤0.6，0≤y≤0.6，0.85≤m≤1.30，且x或y不为零。
玻璃成分包括总量30-70mol％的TiO2和SiO2。另外，玻璃成分包括Li2O、RO、Al2O3，其中R至少是从钯(Ba)、锶(Sr)、钙(Ca)、镁(Mg)中选择的一种元素。
在本发明的烧结陶瓷体中，次生相包含等于或少于30mol％的钙，因而改善了在高温负荷试验中的可靠性。下面描述一个本发明的典型实例。
一个多层陶瓷电容规格是：长2.0mm、宽1.2mm、厚1.2mm，制作程序如下：
首先，将烧制过的CaTiO3和CaZrO3、MnO2粉末，以及含SiO2的细粉末按下面所述内容混合，将有机粘合剂和溶剂加入到该混合物中以制备陶瓷浆。
对于重量百分比100的煅烧过的CaTiO3和CaZrO3，陶瓷原浆包含重量百分比1.0的Si-Li烧结促进剂，重量百分比1.4的MnO2，重量百分比10的粘合剂，重量百分比1.4的可塑剂。
将陶瓷原浆制成在烧制后能具有5.0μm厚度的绿瓷薄片。一些绿瓷薄片被涂覆以镍涂层，形成电极图案。将印制图案的绿瓷薄片叠制，然后在上、下表面分别叠加无图案的绿瓷薄片以形成母叠片。在厚度方向上对母叠片施压，然后切割成绿色瓷叠片用于构成陶瓷电容。每个绿瓷叠片具有位于内部电极之间的10个陶瓷层，因此有11个内部电极。
绿瓷叠片是以下面描述的加热速率条件下煅烧以形成烧结陶瓷体。在这个例子中，最大煅烧温度为1300℃。
加热速率是从下列五种中选择的：(a)1.0℃/min(b)3.0℃/min(c)5.0℃/min(d)10.0℃/min(e)20.0℃/min经滚筒抛光后，将烧结体两端涂覆以铜浆料，然后烘烤以形成外部电极。一个外部电极是用镀镍层给出的，另一个外部电极是用镀锡层给出的。这样，图1所示的多层陶瓷电容器制作全部完成。
多层陶瓷电容器1包括烧结陶瓷体2、置于烧结陶瓷体2中的内部电极3-6。烧结的陶瓷体2的彼此相反的两个面2a和2b、分别有外部电极7和8。
对根据上面所述步骤形成的多层陶瓷电容器进行了高温载荷测试和成分分析。
在高温负荷试验中多层陶瓷电容器经受了在温度150℃，电压100V下的200小时测试，检查其短路和绝缘电阻降低特性。
在成分分析中：针对多层陶瓷电容器的次生相，以扫描电子显微镜(SEM)和x-射线能谱分析仪(EDX)进行了定性分析。结果如表3所示。
表3
| 加热速(℃/min) | Ca(钙) | Si(硅) | Mn(锰) | Ti(钛) | Zr(锆) | 高温负荷试验 |
| 1.0 | 44.341.543.6 | 50.653.550.5 | 1.11.21.1 | 0.50.50.2 | 3.53.34.6 | 40/100 |
| 3.0 | 35.133.233.0 | 58.658.659.0 | 1.31.21.1 | 0.30.40.3 | 4.76.66.6 | 20/100 |
| 5.0 | 30.027.227.5 | 62.163.065.1 | 1.31.31.4 | 0.10.2ND | 6.58.36.0 | 0/100 |
| 10 | 28.025.125.0 | 62.965.766.8 | 1.41.41.3 | NDNDND | 7.77.86.9 | 0/100 |
| 20 | 26.026.724.9 | 64.864.766.8 | 1.41.51.4 | NDNDND | 7.87.16.9 | 0/100 |
表3显示，以加热速率(a)或(b)得到的每个多层陶瓷电容，其在高温负荷试验中表现出短路和绝缘电阻降低。形成对照，以加热速率(c)到(e)得到的每个多层陶瓷电容就未表现出这些缺陷。所以，至少5℃/min的加热速率得到的多层陶瓷电容，几乎不会出现上述的在高温负荷试验中的短路和绝缘电阻降低的缺陷。
次生相的成份分析结果表明，以(c)到(e)加热速率煅烧，导致在次生相中等于或少于30mol％的钙(Ca)含有量。换言之，次生相具有等于或少于30mol％的钙含量的次生相的多层陶瓷电容器就不会出现上述缺陷。
图2表明的是，以加热速率(c)制作的多层陶瓷电容器的次生相状态的示意图。内部电极3和5间的每一陶瓷层主要由主结晶相A构成，次生相B与主结晶相A出现分离。这些次生相B中的钙含有量在本发明中限制为30mol％。
由表3看出，大于或等于5.0℃/min的加热速率导致含有等于或少于30mol％钙的次生相。
通过限制次生相中的钙含有量至30mol％，就可以避免多层陶瓷电容器在高温负荷试验中出现短路和绝缘电阻降低，产生的多层陶瓷电容器具有主要包含CaTiO3和CaZrO3的主结晶相和次生相主要包含钙Ca和硅Si的次生相。
在前面的例子中，镍被用作内部电极，而且也可使用另一贱金属如铜，以降低多层陶瓷电容的材料成本。而且，如银、钯、银-钯合金这样的贵金属也可用作本发明的内部电极。在本发明中使用这样的贵金属，同样可以避免在高温负荷试验中的短路和绝缘电阻降低。
包括贱金属内部电极的绿瓷叠片需要在中性或贫气的环境下煅烧，这对于根据本发明的烧结陶瓷体来说是较好的。
本发明的多层陶瓷电容器具有主要包含CaTiO3、CaZrO3的主结晶相和主要包含钙Ca和硅Si的次生相。次生相的钙含有量限于30mol％内，因此可以避免在高温负荷试验中出现短路和绝缘电阻降低的问题。这些已经根据试验结果被证明。
因此，即使为获得理想的温度特性，能够在中性或还原气氛中烧制的具有高钛(Ti)含量的CaTiO3/CaZrO3烧结体，也将获得在高温负荷试验中很少出现短路和绝缘电阻降低的可靠的多层陶瓷电容。因此，可以稳定地提供具有根据本申请的各种温度特性要求的多层陶瓷电容。
尤其是，当使用贱金属作为内部电极时，包括内部电极的绿瓷叠片需要在中性或还原气氛中烧制，因此最好应用本发明。
在本发明的生产多层陶瓷电容的方法中，是以5.0℃/min的加热速率烧制绿色CaTiO3/CaZrO3陶瓷叠片以形成多层陶瓷电容，因此次生相的钙(Ca)含有量限于30mol％。因此，本发明的多层陶瓷电容器在高温负荷试验中能够具有高可靠性。
Claims (3)
1.一种多层陶瓷电容器，其中包括：
烧结陶瓷体，其包括主要包含CaTiO3和CaZrO3的主结晶相和主要包含钙Ca和硅Si的次生相；
在烧结陶瓷体内放置的内部电极，其中次生相的钙含有量等于或小于30mol％。
2.根据权利要求1所述的多层陶瓷电容器，其特征在于内部电极由贱金属构成。
3.一种制作如权利要求1或2所述多层陶瓷电容器的方法，包括步骤：
制备绿瓷叠片，绿瓷叠片由包括CaTiO3和CaZrO3的主要成分，包括MnO2、SiO2的副成分，以及多个内部电极组成；
以5.0℃/min的加热速率烧制绿瓷叠片，至最高温度。
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| CN103288442A (zh) * | 2012-02-29 | 2013-09-11 | 深圳光启创新技术有限公司 | 一种陶瓷复合材料及其制备的超材料 |
| CN103460316A (zh) * | 2011-09-29 | 2013-12-18 | 株式会社村田制作所 | 层叠陶瓷电容器、以及层叠陶瓷电容器的制造方法 |
| CN104103423B (zh) * | 2013-04-08 | 2017-04-12 | 三星电机株式会社 | 多层陶瓷电容器及其制造方法 |
| CN110218087A (zh) * | 2019-07-05 | 2019-09-10 | 威海市科博乐汽车电子有限公司 | 负温度系数热敏电阻材料的制备方法 |
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| US7173922B2 (en) * | 2000-03-17 | 2007-02-06 | Symbol Technologies, Inc. | Multiple wireless local area networks occupying overlapping physical spaces |
| US7173923B2 (en) * | 2000-03-17 | 2007-02-06 | Symbol Technologies, Inc. | Security in multiple wireless local area networks |
| JP4111006B2 (ja) * | 2003-03-03 | 2008-07-02 | 株式会社村田製作所 | 誘電体セラミックおよびその製造方法ならびに積層セラミックコンデンサ |
| US7428137B2 (en) * | 2004-12-03 | 2008-09-23 | Dowgiallo Jr Edward J | High performance capacitor with high dielectric constant material |
| TWI287811B (en) * | 2005-02-04 | 2007-10-01 | Murata Manufacturing Co | Multilayer ceramic capacitor and method for manufacturing the same |
| US7172985B2 (en) * | 2005-06-07 | 2007-02-06 | Kemet Electronics Corporation | Dielectric ceramic capacitor comprising non-reducible dielectric |
| JP5224074B2 (ja) * | 2010-08-04 | 2013-07-03 | 株式会社村田製作所 | 誘電体セラミック、及び積層セラミックコンデンサ |
| JP5469252B2 (ja) * | 2010-10-01 | 2014-04-16 | 太陽誘電株式会社 | 積層セラミックコンデンサの製造方法 |
| KR101922867B1 (ko) * | 2012-10-12 | 2018-11-28 | 삼성전기 주식회사 | 적층 세라믹 전자부품 및 이의 제조방법 |
| JP7351205B2 (ja) | 2019-12-12 | 2023-09-27 | Tdk株式会社 | 誘電体組成物および電子部品 |
| JP7306251B2 (ja) * | 2019-12-12 | 2023-07-11 | Tdk株式会社 | 誘電体組成物および電子部品 |
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| JPH0831284B2 (ja) | 1986-11-14 | 1996-03-27 | 株式会社村田製作所 | 非還元性温度補償用誘電体磁器組成物 |
| US5258150A (en) * | 1991-12-06 | 1993-11-02 | Corning Incorporated | Fabrication of low thermal expansion, high porosity cordierite body |
| JPH0845343A (ja) * | 1994-07-28 | 1996-02-16 | Kyocera Corp | 誘電体磁器組成物 |
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| JP2001006966A (ja) * | 1999-06-17 | 2001-01-12 | Murata Mfg Co Ltd | セラミックコンデンサおよびその製造方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103460316A (zh) * | 2011-09-29 | 2013-12-18 | 株式会社村田制作所 | 层叠陶瓷电容器、以及层叠陶瓷电容器的制造方法 |
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| CN103288442A (zh) * | 2012-02-29 | 2013-09-11 | 深圳光启创新技术有限公司 | 一种陶瓷复合材料及其制备的超材料 |
| CN103288442B (zh) * | 2012-02-29 | 2016-12-14 | 深圳光启创新技术有限公司 | 一种陶瓷复合材料及其制备的超材料 |
| CN104103423B (zh) * | 2013-04-08 | 2017-04-12 | 三星电机株式会社 | 多层陶瓷电容器及其制造方法 |
| CN110218087A (zh) * | 2019-07-05 | 2019-09-10 | 威海市科博乐汽车电子有限公司 | 负温度系数热敏电阻材料的制备方法 |
| CN110218087B (zh) * | 2019-07-05 | 2021-12-07 | 威海市科博乐汽车电子有限公司 | 负温度系数热敏电阻材料的制备方法 |
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| CN1212629C (zh) | 2005-07-27 |
| JP2002265261A (ja) | 2002-09-18 |
| TW548665B (en) | 2003-08-21 |
| KR20020071780A (ko) | 2002-09-13 |
| US6487065B1 (en) | 2002-11-26 |
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