CN106747418A - 一种具有抗还原性的高介瓷介电容器材料 - Google Patents

一种具有抗还原性的高介瓷介电容器材料 Download PDF

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CN106747418A
CN106747418A CN201611130827.XA CN201611130827A CN106747418A CN 106747418 A CN106747418 A CN 106747418A CN 201611130827 A CN201611130827 A CN 201611130827A CN 106747418 A CN106747418 A CN 106747418A
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ceramic capacitor
mlcc
jie
reduction
resistance
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杨魁勇
程华容
韩敬
孙淑英
宋蓓蓓
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Beijing Yuan Six Hongyuan Electronic Polytron Technologies Inc
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Abstract

本发明公开了一种具有抗还原性的高介瓷介电容器材料，该材料由主料和改性剂组成，主料为BaTiO3，改性剂为BaCO3、MnCO3、SiO2、Mg(OH)2、Y2O3和Dy2O3；以及Nb2O5、CaCO3和Al2O3中的一种或多种；其中，按重量份计：BaTiO3为100份，BaCO3为1.00～2.50份、MnCO3为0.08～0.25份、SiO2为1.00～1.80份、Mg(OH)2为0.15～0.25份、Y2O3为0.65～0.95份，Dy2O3为0.25～0.45份；Nb2O5为0～0.40份、CaCO3为0～0.25份，Al2O3为0～0.05份。本发明通过上述组分制备的电容器材料同时具备高介电常数、低损耗和绝缘电阻率高的优点，采用该材料试生产镍电极多层瓷介电容器(MLCC)，其流延工艺性良好，适应还原性气氛烧结，MLCC的温度特性满足X7R，且具有介电常数高(ε＞3500)、损耗低、绝缘电阻率高和烧结温度低(1200℃～1240℃)等优点。

Description

一种具有抗还原性的高介瓷介电容器材料
技术领域
本发明涉及电容器技术领域，尤其涉及一种具有抗还原性的高介瓷介电容器材料，该材料可用于贱金属内电极MLCC的生产。
背景技术
MLCC被广泛应用于各种电子整机中的旁路、滤波、调谐、振荡、耦合电路，尤其在计算机电源网络、移动通讯设备和汽车电子设备等领域，其需求量巨大。随着对MLCC小尺寸、高容量要求的提出，MLCC介质层将不断地增加，内电极的面积也将不断的增加，导致MLCC的生产成本增加，MLCC的内电极贱金属化成为必然的发展趋势。
目前，主要发展的MLCC内电极为Ni、Cu等贱金属及其合金。而这些贱金属在空气中烧结会发生氧化，失去作为内电极的作用，故必须使用中性或还原性气氛烧结。但在低氧分压条件下烧结时，BaTiO3材料体系中部分钛离子从4价还原成3价，晶体结构中形成了氧空位，而晶格上的3价钛不稳定，最终导致材料半导体化，绝缘电阻下降。开发并生产抗还原性的陶瓷材料成为MLCC贱金属化的关键环节。
现已公开的涉及抗还原瓷介电容器材料的文献很多，但能够同时兼具综合性能优异、成本低和工业化可实现性强的材料，鲜见报道。如发明公开号CN101182201A中的改性剂采用溶胶凝胶法进行加工，其工艺复杂、产率低、原材料成本高、工业化实现困难；CN101183610A和CN101880167A化学共沉淀法，合成包覆钛酸钡粉体，该方法过程控制严格，工业化实现困难。
发明内容
针对上述问题中存在的不足之处，本发明提供一种具有抗还原性的高介瓷介电容器材料。
为实现上述目的，本发明提供一种具有抗还原性的高介瓷介电容器材料，该材料由主料和改性剂组成，其中：
所述主料为BaTiO3；
所述改性剂为BaCO3、MnCO3、SiO2、Mg(OH)2、Y2O3和Dy2O3；以及Nb2O5、CaCO3和Al2O3中的一种或多种。
作为本发明的进一步改进，按重量份计：
所述BaTiO3为100份，所述BaCO3为1.00～2.50份、所述MnCO3为0.08～0.25份、所述SiO2为1.00～1.80份、所述Mg(OH)2为0.15～0.25份、所述Y2O3为0.65～0.95份，所述Dy2O3为0.25～0.45份；所述Nb2O5为0～0.40份、所述CaCO3为0～0.25份，所述Al2O3为0～0.05份。
作为本发明的进一步改进，所述BaTiO3为高结晶度的四方相结构钛酸钡，其纯度≥99.8wt％，粒度D50为0.65～0.80μm。
与现有技术相比，本发明的有益效果为：
本发明公开的一种具有抗还原性的高介瓷介电容器材料，通过上述组分制备的电容器材料同时具备高介电常数、低损耗和绝缘电阻率高的优点，采用该材料试生产镍电极多层瓷介电容器(MLCC)，其流延工艺性良好，适应还原性气氛烧结，MLCC的温度特性满足X7R，且具有介电常数高(ε＞3500)、损耗低、绝缘电阻率高和烧结温度低(1200℃～1240℃)等优点；本发明所涉及的材料为抗还原型瓷介电容器材料，可用于贱金属内电极的MLCC生产，该材料进行了MLCC的工艺验证(流延膜片厚度10μm±0.3μm)，流延及烧结等工艺性良好，所生产的MLCC的综合性能优异，本发明所提供的具有抗还原的高介瓷介电容器材料具有良好的发展和产业化前景。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明所选原料如无特殊说明，均可通过商业渠道采购。
本发明提供一种具有抗还原性的高介瓷介电容器材料，采用该材料制作的瓷介电容器能够实现还原气氛烧结，并保持良好介电性能、较低的损耗、较高的绝缘电阻率和高击穿电压以及良好的温度特性。其中：
本发明提供一种具有抗还原性的高介瓷介电容器材料，该材料由主料和改性剂组成；
主料为BaTiO3，BaTiO3为结晶度较高的的四方相结构钛酸钡，其纯度≥99.8wt％，粒度D50为0.65～0.80μm，便于保障该材料良好的电性能、实现电容器制造并保证电容器的高可靠性。
改性剂为BaCO3、MnCO3、SiO2、Mg(OH)2、Y2O3和Dy2O3；以及Nb2O5、CaCO3和Al2O3中的一种或多种；其中：
按重量份计：
BaTiO3的质量分数为93.55wt％-96.97wt％，其中，该材料以100重量份的钛酸钡为基材，各成分及相对含量如下：BaTiO3为100份，BaCO3为1.00～2.50份、MnCO3为0.08～0.25份、SiO2为1.00～1.80份、Mg(OH)2为0.15～0.25份、Y2O3为0.65～0.95份，Dy2O3为0.25～0.45份；Nb2O5为0～0.40份、CaCO3为0～0.25份，Al2O3为0～0.05份。
本发明一种具有抗还原性的高介瓷介电容器材料的制备步骤包括：称量、球磨、烘干和过筛；
其中，按所设计的重量比例称取主料和改性剂于球磨罐中；以去离子水为介质进行混合球磨，为时2～5小时；烘干温度为110～120℃，烘干时间6～8小时；采用玛瑙研钵处理后，过筛目数为40，之后密封储存备用。
为验证圆片性能，本发明具有抗还原性的高介瓷介电容器材料烧制成陶瓷圆片样品，需进行以下处理：
步骤1、将材料进行造粒、压片，制成陶瓷生坯圆片；
步骤2、将陶瓷生坯圆片放入电阻炉中，以2～3℃/min由室温升高到500～600℃，保温2～3小时，排出其中的有机物；
步骤3、将陶瓷圆片样品放入气氛炉中进行烧结，其烧结曲线包括：升温段、高温段、再氧化段和降温段；其中，升温段(500℃～1200℃)和高温段(1200℃～1240℃)通入含H2的N2，再氧化段(1000℃～700℃)通入含O2的N2，降温段(700℃至室温)通入空气。
步骤4、将陶瓷圆片样品进行表面处理，涂覆并烧制电极。
为验证该材料用于生产MLCC的工艺性，由该材料经配料、流延、印刷、叠层、匀压、排胶、烧结、倒角、涂端、烧端、电镀获得MLCC芯片，并测试性能。
本发明公开的一种具有抗还原性的高介瓷介电容器材料，通过上述组分制备的电容器材料同时具备高介电常数、低损耗和绝缘电阻率高的优点，采用该材料试生产镍电极多层瓷介电容器(MLCC)，其流延工艺性良好，适应还原性气氛烧结，MLCC的温度特性满足X7R，且具有介电常数高(ε＞3500)、损耗低、绝缘电阻率高和烧结温度低(1200℃～1240℃)等优点。
本发明具有抗还原性的高介瓷介电容器材料采用传统固相法制备，该方法工艺简单，成本低，易于实现工业化生产，能够获得综合性能优异的陶瓷材料。1、圆片样品：室温相对介电常数为2200～2400，室温损耗≤1.0％，室温绝缘电阻率(2.0～3.6)×1012Ω·cm；2、采用该陶瓷材料进行流延(本发明采用厚度为10μm膜进行工艺验证，在实际生产中不仅限于10μm膜片)，试生产尺寸为1210，容量为5.0μF的MLCC，其反推介电常数ε＝3500～3600，损耗≤3.0％，C·R＞2500μF·MΩ，击穿强度＞40v/μm，温度特性满足X7R；本发明所涉及的材料为抗还原型瓷介电容器材料，可用于贱金属内电极的MLCC生产，该材料进行了MLCC的工艺验证(流延膜片厚度10μm±0.3μm)，流延及烧结等工艺性良好，所生产的MLCC的综合性能优异，本发明所提供的具有抗还原的高介瓷介电容器材料具有良好的发展和产业化前景。
实施例1：
本发明提供一种具有抗还原性的高介瓷介电容器材料，由主料和改性剂构成；其中，主料为四方相BaTiO3，粒度D50＝0.65μm，纯度≥99.8wt％。
按照表1的重量比进行主料和改性剂的称取(单位为克)，以去离子水为介质，球磨混合5小时，在120℃下烘干6小时，取出陶瓷粉体，研磨并过40目筛后，用自封袋进行封装储存。
表1
对所制备材料进行性能考核：称取3g粉体材料，加入6.5wt％的PVA水溶液进行造粒，在200MPa下压制成Ф＝10mm的圆片，在还原气氛中烧结，随炉冷却后，进行样品表面处理，并涂覆、烧结电极。制成圆片电容器后测试容值、损耗、绝缘电阻和击穿电压，并计算得出相对介电常数、绝缘电阻率和击穿场强；并测试其温度特性，其电学性能参数见表2。
表2
采用配方3和配方6对应的陶瓷材料，经配料、流延、印刷、叠层、匀压、排胶、烧结(烧结温度1210℃)、倒角、涂端、烧端、电镀获得尺寸规格为1210、容量为5.0μF的MLCC芯片(平均介质层厚度8.3μm)；MLCC电学性能如表3所示。
表3
实施例2：
本发明提供一种具有抗还原性的高介瓷介电容器材料，由主料和改性剂构成；其中，主料为四方相BaTiO3，粒度D50＝0.75μm，纯度≥99.8wt％。
表4
材料组份 配方7 配方8 配方9 配方10 配方11 配方12
BaTiO3 100 100 100 100 100 100
BaCO3 2.15 1.95 1.50 1.00 2.50 1.55
MnCO3 0.20 0.14 0.14 0.20 0.15 0.08
SiO2 1.45 1.50 1.80 1.35 1.10 1.40
CaCO3 0.10 0.05 0 0.10 0 0
Mg(OH)2 0.20 0.25 0.19 0.15 0.20 0.19
Y2O3 0.86 0.85 0.85 0.83 0.80 0.65
Al2O3 0.05 0.02 0.04 0.04 0.04 0.03
Dy2O3 0.28 0.32 0.30 0.28 0.35 0.45
按照表4的重量比进行主料和改性剂的称取(单位为克)，以去离子水为介质，球磨混合5小时，在120℃下烘干6小时，取出陶瓷粉体，研磨并过40目筛后，用自封袋进行封装储存。
对所制备材料进行性能考核：称取3g陶瓷粉体，加入6.5wt％的PVA水溶液进行造粒，在200MPa下压制成Ф＝10mm的圆片，在还原气氛中烧结，随炉冷却后，进行样品表面处理，并涂覆、烧结电极。制成圆片电容器后测试容值、损耗、绝缘电阻和击穿电压，并计算得出相对介电常数、绝缘电阻率和击穿场强；并测试其温度特性，其电学性能参数见表5。
表5
采用配方10和配方11对应的陶瓷材料，经配料、流延(膜片厚度10.5μm)、印刷、叠层、匀压、排胶、烧结(烧结温度1225℃)、倒角、涂端、烧端、电镀获得尺寸规格为1210、容量为5.0μF的MLCC芯片(平均介质层厚度8.4μm)；MLCC电学性能如表6所示。
表6
本发明公开的一种具有抗还原性的高介瓷介电容器材料，通过上述组分制备的电容器材料同时具备高介电常数、低损耗和绝缘电阻率高的优点，采用该材料试生产镍电极多层瓷介电容器(MLCC)，其流延工艺性良好，适应还原性气氛烧结，MLCC的温度特性满足X7R，且具有介电常数高(ε＞3500)、损耗低、绝缘电阻率高和烧结温度低(1200℃～1240℃)等优点；本发明所涉及的材料为抗还原型瓷介电容器材料，可用于贱金属内电极的MLCC生产，该材料进行了MLCC的工艺验证(流延膜片厚度10μm±0.3μm)，流延及烧结等工艺性良好，所生产的MLCC的综合性能优异，本发明所提供的具有抗还原的高介瓷介电容器材料具有良好的发展和产业化前景。
以上仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (3)

1.一种具有抗还原性的高介瓷介电容器材料，其特征在于，该材料由主料和改性剂组成，其中：
所述主料为BaTiO3；
所述改性剂为BaCO3、MnCO3、SiO2、Mg(OH)2、Y2O3和Dy2O3；以及Nb2O5、CaCO3和Al2O3中的一种或多种。
2.如权利要求1所述的具有抗还原性的高介瓷介电容器材料，其特征在于，按重量份计：
所述BaTiO3为100份，所述BaCO3为1.00～2.50份、所述MnCO3为0.08～0.25份、所述SiO2为1.00～1.80份、所述Mg(OH)2为0.15～0.25份、所述Y2O3为0.65～0.95份，所述Dy2O3为0.25～0.45份；所述Nb2O5为0～0.40份、所述CaCO3为0～0.25份，所述Al2O3为0～0.05份。
3.如权利要求1所述的具有抗还原性的高介瓷介电容器材料，其特征在于，所述BaTiO3为高结晶度的四方相结构钛酸钡，其纯度≥99.8wt％，粒度D50为0.65～0.80μm。
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