CN108083795B - 低温烧结的温度稳定x8r型mlcc介质材料 - Google Patents

低温烧结的温度稳定x8r型mlcc介质材料 Download PDF

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CN108083795B
CN108083795B CN201810105535.3A CN201810105535A CN108083795B CN 108083795 B CN108083795 B CN 108083795B CN 201810105535 A CN201810105535 A CN 201810105535A CN 108083795 B CN108083795 B CN 108083795B
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杨魁勇
程华容
宋蓓蓓
齐世顺
刘佳翔
孙淑英
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BEIJING YUANLIU HONGYUAN ELECTRONIC TECHNOLOGY CO LTD
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Abstract

本发明公开了一种低温烧结的温度稳定X8R型MLCC介质材料，所述温度稳定X8R型MLCC介质材料由主料、副料、改性剂和烧结助剂烧结而成；其中，所述主料为BaTiO3；所述副料为Na0.5Bi0.5TiO3和CaTiO3；所述改性剂包括Nb2O5、MnCO3、Co2O3和MgO。通过本发明的技术方案，保持了良好介电性能、较低的损耗、较高的绝缘电阻率和良好的X8R温度稳定性，且原材料成本低、生产工艺简单、烧结工艺易于控制，符合环保要求，具有良好的实用价值和市场前景。

Description

低温烧结的温度稳定X8R型MLCC介质材料
技术领域
本发明涉及陶瓷组合物技术领域，尤其涉及一种低温烧结的温度稳定X8R型MLCC介质材料。
背景技术
目前，MLCC(Multi-layer Ceramic Capacitors，片式多层陶瓷电容器)是现代电子行业中最广泛应用的被动电子元器件之一，而在航空航天、汽车工业、勘探和军用移动通讯领域，需要承受高温的MLCC，尤其是汽车电子市场已成为全球电容产品的一个新兴需求领域，对高温MLCC的需求量将持续增长。
根据国际电子工业协会EIA标准，X8R温度稳定型MLCC是指以25℃的电容值为基准，在-55℃到+150℃的温度范围之内，其容量温变化率(TCC)≤±15％。目前，大多数的X8R温度稳定型MLCC烧结温度不低于1150℃，需要Ag-Pd电子浆料作为内电极(其中钯含量30％-40％)，因钯含量高导致其生产成本急剧增加。
发明内容
针对上述问题，本发明提供了一种低温烧结的温度稳定X8R型MLCC介质材料，该材料由主料、副料、改性剂和烧结助剂烧结而成；其中，所述主料为BaTiO3；所述副料为Na0.5Bi0.5TiO3和CaTiO3；所述改性剂包括Nb2O5、MnCO3、Co2O3和MgO；以100重量份的所述主料BaTiO3为基础，各成分及相对含量如下：主料BaTiO3为100份；副料Na0.5Bi0.5TiO3为6.50～10.50份；副料CaTiO3为0.50～1.20份；改性剂Nb2O5为1.10～1.50份；改性剂MnCO3为0.10～0.25份；改性剂Co2O3为0.10～0.15份；改性剂MgO为0.02～0.08份；烧结助剂为5.5～9.5份。
进一步的，所述改性剂为Nb2O5、MnCO3、CeO2、Co2O3、ZrO2和MgO中的四种或四种以上。
进一步的，所述改性剂还包括0～0.15份的ZrO2。
进一步的，所述改性剂还包括0～0.05份的CeO2。
进一步的，所述MLCC介质材料为粉末状，粒径为0.7-1.5微米。
进一步的，所述主料BaTiO3的原料粒径为0.6-1.1微米。
进一步的，所述烧结助剂BZBS为B2O3、ZnO、Bi2O3和SiO2中的三种或四种。
进一步的，所述烧结助剂BZBS按照25wt％～40wt％H3BO3、20wt％～35wt％ZnO、30wt％～45wt％Bi2O3和0～10wt％SiO2份量称取，以去离子水为介质，球磨5～8小时，70℃～90℃烘干，研磨后过60目筛，在580℃～650℃下煅烧，自然冷却后，过60目筛，装袋备用。
进一步的，将上述各成分按照重量份数称取，放入装有氧化锆(ZrO2)球的球磨罐中，加上适量的去离子水球磨、烘干、研磨后过40目筛，装袋备用。
进一步的，所述MLCC介质材料的烧结温度为930～980℃。
进一步的，所述MLCC介质材料的制备原料均采用分析纯的原料。
与现有技术相比，本发明的有益效果为：介质材料具备粒度分布均匀、分散性好、成型性工艺好，烧结温度降至930℃～980℃，能够与低钯的银钯内电极或纯银内电极共烧，具有高介电常数(ε＝1700～1950)、较低损耗(tanδ≤1.80％)、较高绝缘电阻率(≥1.5×1012Ω·cm)、温度特性满足X8R要求，且原材料成本低、生产工艺简单、烧结工艺易于控制，不含Pb、Cd、Hg、Cr等有毒元素，符合环保要求，生产出的MLCC性能优良、成本低，具有良好的实用价值和市场前景。
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，下面将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。
下面对本发明做进一步的详细描述：
根据本发明提供的一种低温烧结的温度稳定X8R型MLCC介质材料，由主料、副料、改性剂和烧结助剂烧结而成，其中：主料为BaTiO3；副料为Na0.5Bi0.5TiO3和CaTiO3；改性剂包括Nb2O5、MnCO3、Co2O3和MgO。该介质材料以100重量份的BaTiO3为基材，各成分及相对含量如下：主料BaTiO3为100份；副料Na0.5Bi0.5TiO3为6.50～10.50份；副料CaTiO3为0.50～1.20份；改性剂Nb2O5为1.10～1.50份；改性剂MnCO3为0.10～0.25份；改性剂Co2O3为0.10～0.15份；改性剂MgO为0.02～0.08份；烧结助剂为5.5～9.5份。
进一步的，改性剂为Nb2O5、MnCO3、CeO2、Co2O3、ZrO2和MgO中的四种或四种以上。
进一步的，改性剂还包括0～0.15份的ZrO2。
进一步的，改性剂还包括0～0.05份的CeO2。
进一步的，所述MLCC介质材料为粉末状，粒径为0.7-1.5微米。
进一步的，所述主料BaTiO3的原料粒径为0.6-1.1微米。
进一步的，所述烧结助剂BZBS为B2O3、ZnO、Bi2O3和SiO2中的三种或四种。具体的，烧结助剂BZBS按照25wt％～40wt％H3BO3、20wt％～35wt％ZnO、30wt％～45wt％Bi2O3和0～10wt％SiO2份量称取，以去离子水为介质，球磨5～8小时，70℃～90℃烘干，研磨后过60目筛，在580℃～650℃下煅烧，自然冷却后，过60目筛，装袋备用。
进一步的，一种用于低温烧结的温度稳定X8R型MLCC介质材料，主料BaTiO3粒度D50为0.60μm～1.10μm，烧结完成后的X8R型MLCC介质中BaTiO3占总成份重量的85wt％-90wt％。
进一步的，上述用于低温烧结的温度稳定X8R型MLCC介质材料的制备方法为：将上述主料、副料、改性剂和烧结助剂按照重量称取后放入装有氧化锆球的球磨罐中；加入适量的去离子水进行球磨、烘干、研磨，并将研磨后的粉末后过40目筛；将过筛后的介质材料加入6.5wt％的PVA(polyvinyl alcohol，聚乙烯醇)水溶液进行造粒；将造粒后的陶瓷坯体压制成圆片，在空气中按照一定的烧结曲线进行烧结，烧结后随炉自然冷却至室温。
具体地，以下述实施例对本发明提出的低温烧结的温度稳定X8R型MLCC介质材料进行详细描述：
实施例1
一种用于低温烧结的温度稳定X8R型MLCC介质材料，由主料、副料、改性剂和烧结助剂构成。其中，主料BaTiO3粒度D50＝0.60μm，纯度≥99.8％。
按照摩尔比1.01：1.01：4称取分析纯的Bi2O3、Na2CO3和TiO2，并以无水乙醇为介质，球磨10小时，在80℃下烘干，研磨并过120目筛，在850℃下煅烧2.5小时，得到Na0.5Bi0.5TiO3粉体，并用自封袋进行封装储存备用。
按照摩尔比1:1称取分析纯的CaCO3和TiO2，并以去离子水为介质，球磨8小时，在120℃烘干，研磨并过80目筛，在1060℃下煅烧3小时，得到CaTiO3粉体，并用自封袋进行封装储存备用。
按照30wt％H3BO3、25wt％ZnO和45wt％Bi2O3称取，以去离子水为介质，球磨5～8小时，70℃～90℃烘干，研磨后过60目筛，在580℃下煅烧，自然冷却后，过60目筛，制得烧结助剂BZB，装袋备用。
按照表1的重量比进行主料、副料、改性剂和烧结助剂的称取(单位为克)，以去离子水为介质，球磨5小时，在120℃下烘干，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介质材料配方
材料组份 配方1 配方2 配方3 配方4 配方5 配方6
BaTiO<sub>3</sub> 100.00 100.00 100.00 100.00 100.00 100.00
Na<sub>0.5</sub>Bi<sub>0.5</sub>TiO<sub>3</sub> 6.50 6.50 7.50 9.00 10.00 10.50
CaTiO<sub>3</sub> 0.95 1.20 0.78 0.70 0.64 0.50
Nb<sub>2</sub>O<sub>5</sub> 1.10 1.15 1.30 1.35 1.35 1.45
MnCO<sub>3</sub> 0.15 0.15 0.10 0.20 0.25 0.25
CeO<sub>2</sub> 0.02 0.02 0 0 0.05 0.05
Co<sub>2</sub>O<sub>3</sub> 0.13 0.12 0.10 0.11 0.15 0.15
MgO 0.03 0.03 0.02 0.04 0.08 0.06
BZB 6.50 6.50 7.50 7.00 8.50 9.50
对所制备陶瓷材料进行性能考核：称取陶瓷粉体，加入6.5wt％的PVA水溶液进行造粒，压制成圆片，在空气中进行烧结，其烧结曲线为：由室温以2.5℃/min升至560℃，并保温3小时；再以5℃/min升至930℃，保温2.5小时，之后随炉自然冷却降至室温。将烧制完的陶瓷圆片的两表面涂覆银浆、烧制银电极，制成圆片电容器后测试容值、损耗、绝缘电阻和温度特性，并计算相对介电常数和绝缘电阻率，其电学性能参数见表2。
表2介质材料圆片性能
Figure GDA0002489702230000051
实施例2
一种用于低温烧结的温度稳定X8R型MLCC介质材料，由主料、副料、改性剂和烧结助剂构成。其中，主料BaTiO3粒度D50＝1.10m，纯度≥99.8％。
按照摩尔比1.01：1.01：4称取分析纯的Bi2O3、Na2CO3和TiO2，并以无水乙醇为介质，球磨10小时，在80℃下烘干，研磨并过120目筛，在850℃下煅烧2.5小时，得到Na0.5Bi0.5TiO3粉体，并用自封袋进行封装储存备用。
按照摩尔比1:1称取分析纯的CaCO3和TiO2，并以去离子水为介质，球磨8小时，在120℃烘干，研磨并过80目筛，在1060℃下煅烧3小时，得到CaTiO3粉体，并用自封袋进行封装储存备用。
按照25wt％H3BO3、30wt％ZnO、35wt％Bi2O3和10wt％SiO2称取，以去离子水为介质，球磨5～8小时，90℃烘干，研磨后过60目筛，在650℃下煅烧，自然冷却后，过60目筛，制得烧结助剂BZBS，装袋备用。
按照表3的重量比进行主料、副料、改性剂和烧结助剂的称取(单位为克)，以去离子水为介质，球磨5小时，在120℃下烘干，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3介质材料配方组份
Figure GDA0002489702230000052
Figure GDA0002489702230000061
对所制备陶瓷材料进行性能考核：称取陶瓷粉体，加入6.5wt％的PVA水溶液进行造粒，在200MPa下压制成直径Ф＝10mm的圆片，在空气中进行烧结，其烧结曲线为：由室温以2.5℃/min升至560℃，并保温3小时；再以5℃/min升至980℃，保温2.5小时，随炉自然冷却降至室温。将烧制完的陶瓷圆片的两表面涂覆银浆、烧制银电极，制成圆片电容器后测试容值、损耗、绝缘电阻和温度特性，并计算相对介电常数和绝缘电阻率，其电学性能参数见表4。
表4介质材料圆片性能
Figure GDA0002489702230000062
以上所述为本发明的实施方式，根据上述实施例的制备和测试数据可以看出，本发明提出的低温烧结的温度稳定X8R型MLCC介质材料，其烧结温度在930℃至980℃，能够使用低钯的Ag-Pd电子浆料(钯含量不高于5％)甚至纯银内电极，保持了良好介电性能、较低的损耗、较高的绝缘电阻率和良好的X8R温度稳定性，且原材料成本低、生产工艺简单、烧结工艺易于控制，不含Pb、Cd、Hg、Cr等有毒元素，符合环保要求，具有良好的实用价值和市场前景。
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 (8)

1.一种低温烧结的温度稳定X8R型MLCC介质材料，其特征在于：
所述温度稳定X8R型MLCC介质材料由主料、副料、改性剂和烧结助剂烧结而成；其中，
所述主料为BaTiO3；
所述副料为Na0.5Bi0.5TiO3和CaTiO3；
所述改性剂包括Nb2O5、MnCO3、Co2O3和MgO；
以100重量份的所述主料BaTiO3为基础，各成分及相对含量如下：
主料BaTiO3为100份；
副料Na0.5Bi0.5TiO3为6.50～10.50份；
副料CaTiO3为0.50～1.20份；
改性剂Nb2O5为1.10～1.50份；
改性剂MnCO3为0.10～0.25份；
改性剂Co2O3为0.10～0.15份；
改性剂MgO为0.02～0.08份；
烧结助剂为5.5～9.5份；
所述烧结助剂为B2O3、ZnO、Bi2O3和SiO2中的三种或四种；
所述烧结助剂的成分为25wt％～40wt％的H3BO3、20wt％～35wt％的ZnO、30wt％～45wt％的Bi2O3和0～10wt％的SiO2。
2.根据权利要求1所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述改性剂还包括CeO2和/或ZrO2。
3.根据权利要求1所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述改性剂还包括0～0.15份的ZrO2。
4.根据权利要求1或3所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述改性剂还包括0～0.05份的CeO2。
5.根据权利要求1所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述MLCC介质材料为粉末状，粒径为0.7-1.5微米。
6.根据权利要求1所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述主料BaTiO3的原料粒径为0.6-1.1微米。
7.根据权利要求1所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述MLCC介质材料的烧结温度为930～980℃。
8.根据权利要求1所述的低温烧结的温度稳定X8R型MLCC介质材料，其特征在于，所述MLCC介质材料的制备原料均采用分析纯的原料。
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