CN108610041A - 一种提高钛锡酸钡在还原气氛下介电性能的方法 - Google Patents

一种提高钛锡酸钡在还原气氛下介电性能的方法 Download PDF

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CN108610041A
CN108610041A CN201810394450.1A CN201810394450A CN108610041A CN 108610041 A CN108610041 A CN 108610041A CN 201810394450 A CN201810394450 A CN 201810394450A CN 108610041 A CN108610041 A CN 108610041A
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李玲霞
王瑞杰
于仕辉
孙正
张宁
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Abstract

本发明公开了一种提高钛锡酸钡在还原气氛下介电性能的方法，先将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1‑x)O3其中0＜x≤0.3的化学式称量配料，经球磨、烘干、过筛后于1000～1300℃下煅烧，合成主晶相；再经二次球磨、烘干，过筛后外加质量百分比为7％的粘结剂，进行造粒，再将造粒粉料压制成生坯，生坯经排胶后，在还原气氛下，于1300～1450℃烧结，制得高介电常数低损耗低频钛锡酸钡介质材料。本发明的介电常数从2000提高到24000，可用于多层片式陶瓷电容器(MLCC)的制备，大大提高了电容器器件的介电性能。

Description

一种提高钛锡酸钡在还原气氛下介电性能的方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种提高钛锡酸钡在还原气氛下的介电性能的制备方法。
背景技术
MLCC(多层片式陶瓷电容器)的制作工艺要求内电极必须与介质材料进行共同烧结以形成独石结构，而常见的MLCC瓷料如BaTiO3系统瓷料的烧结温度较高，对于通常的空气气氛烧结而言，只有那些熔点高、难氧化、具有低电阻率的金属才能作为内电极材料，一般选用贵金属Pt、Pd或Pd-Ag合金作为MLCC内电极，这样在MLCC的生产成本中内电极材料成本占了较大比例，并一度造成MLCC的成本因电极材料昂贵而居高不下，极大地限制了其应用范围。此外，MLCC的大比容化要求减小介质层的厚度并增加陶瓷介质的层数，但是随着介质层数的增加，内电极层数也相应增加，更导致MLCC的生产成本提高。因此，MLCC的低成本化迫切要求内电极贱金属化。当选用Ni电极作为金属电极时，就要求介质材料和电极同时在还原气氛中共烧，进而要求介质材料的抗还原性。
随着电子信息技术的不断发展，为了实现电子产品给生活带来更多便捷，电子产品逐渐小型化和大容量。为了实现这一目标，就要求介质材料具有更高的介电常数，进而实现相同体积的MLCC能够有更大的容量。
Ba(SnxTi1-x)O3介质材料是一类很重要的电子陶瓷材料。一方面，它的应用很广泛，可以作为高介电容器、介质放大器、参量器件以及开关电路保护器等。另一方面，随着Sn含量的增加，Ba(SnxTi1-x)O3陶瓷会表现出从典型铁电体到弛豫型铁电体的过渡，所以，它是一类对于铁电体物理学的理论研究很重要的材料。
发明内容
本发明的目的，是在现有技术的基础上进一步提高其介电性能，提供一种钛锡酸钡在还原气氛下烧结以提高介电性能的方法。
本发明通过如下技术方案予以实现。
一种提高钛锡酸钡在还原气氛下介电性能的方法，具有如下步骤：
(1)将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1-x)O3，其中0＜x≤0.3的化学式称量配料；
(2)将步骤(1)配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1000～1300℃下煅烧3小时，合成主晶相；
(4)将步骤(3)合成主晶相的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(5)在步骤(4)处理后的粉料中外加质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料压制成生坯，经排胶后，在还原气氛下，于1300～1450℃烧结，保温2～4小时，制得高介电常数低损耗低频钛锡酸钡介质材料。
所述步骤(2)的烘干温度为100℃。
所述步骤(2)的粉料与氧化锆球、去离子水的质量比为1∶1∶2。
所述步骤(5)的坯体为Φ10mm×1mm的圆片。
所述步骤(5)的烧结温度为1400℃。
本发明提供了一种钛锡酸钡介质材料在还原气氛下提高介电性能的方法。通过调整x的值以及烧结温度，制得的Ba(SnxTi1-x)O3介质材料(其中x＝0～0.23)，其烧结温度为1300～1450℃，介电常数从2000提高到24000，可用于多层片式陶瓷电容器(MLCC)的制备，大大提高多层片式陶瓷电容器器件的性能。
具体实施方式
下面通过具体实施例对本发明作进一步说明，实例中所用原料均为市售分析纯试剂，具体实施例如下。
实施例1
(1)将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1-x)O3化学式称量配料(x＝0.05)；
(2)将上述配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，粉体与氧化锆球、去离子水的质量比为1∶1∶2；再将球磨后的原料置于红外干燥箱中于100℃下烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1050℃下煅烧3小时，合成主晶相；
(4)将步骤(3)中合成主晶相的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(5)在步骤(4)处理后的粉料加入质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料用用粉末压片机以6MPa的压力压成Φ10mm×1mm的坯体，经排胶后，于1350℃烧结，保温3小时，制得高介电常数低损耗低频钛锡酸钡介质材料。
(7)采用TH2828S测试其制品的电容量C，计算出制品的介电常数和1KHz下εr＝2611.278326。
实施例2
(1)将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1-x)O3化学式称量配料(x＝0.15)；
(2)将上述配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，粉体与氧化锆球、去离子水的质量比为1∶1∶2；将球磨后的原料置于红外干燥箱中于100℃下烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1050℃下煅烧3小时，合成主晶相；
(4)将步骤(3)中合成主晶相的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(5)在步骤(4)处理后的粉料加入质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料用用粉末压片机以6MPa的压力压成Φ10mm×1mm的坯体，经排胶后，于1450℃烧结，保温3小时，制得高介电常数低损耗低频钛锡酸钡介质材料。
(7)采用TH2828S测试其制品的电容量C，计算出制品的介电常数和1KHz下εr＝24373.71。
实施例3
(1)将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1-x)O3化学式称量配料(x＝0.25)；
(2)将上述配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，粉体与氧化锆球、去离子水的质量比为1∶1∶2；将球磨后的原料置于红外干燥箱中于100℃下烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1050℃下煅烧3小时，合成主晶相；
(4)将步骤(3)中合成主晶相的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(5)在步骤(4)处理后的粉料加入质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料用用粉末压片机以6MPa的压力压成Φ10mm×1mm的坯体，经排胶后，于1450℃烧结，保温3小时，制得高介电常数低损耗低频钛锡酸钡介质材料。
(7)采用TH2828S测试其制品的电容量C，计算出制品的介电常数和1KHz下εr＝2648.37。
实施例4
(1)将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1-x)O3化学式称量配料(x＝0.3)；
(2)将上述配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，粉体与氧化锆球、去离子水的质量比为1∶1∶2；将球磨后的原料置于红外干燥箱中于100℃下烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1050℃下煅烧3小时，合成主晶相；
(4)将步骤(3)中合成主晶相的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(5)在步骤(4)处理后的粉料加入质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料用用粉末压片机以6MPa的压力压成Φ10mm×1mm的坯体，经排胶后，于1400℃烧结，保温3小时，制得高介电常数低损耗低频钛锡酸钡介质材料。
(7)采用TH2828S测试其制品的电容量C，计算出制品的介电常数和1KHz下εr＝1213.945922。
具体实施例的相关工艺参数与介电性能详见表1。除表1中的数值区别之外，实施例1～4之外的具体实施例的工艺过程与实施例1～4完全相同。
表1
本发明不局限于上述实施例，一些细节的变化是可能的，但这并不因此违背本发明的范围和精神。

Claims (5)

1.一种提高钛锡酸钡在还原气氛下介电性能的方法，具有如下步骤：
(1)将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1-x)O3，其中0＜x≤0.3的化学式称量配料；
(2)将步骤(1)配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1000～1300℃下煅烧3小时，合成主晶相；
(4)将步骤(3)合成主晶相的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(5)在步骤(4)处理后的粉料中外加质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料压制成生坯，经排胶后，在还原气氛下，于1300～1450℃烧结，保温2～4小时，制得高介电常数低损耗低频钛锡酸钡介质材料。
2.根据权利要求1所述的一种提高钛锡酸钡在还原气氛下介电性能的方法，其特征在于，所述步骤(2)的烘干温度为100℃。
3.根据权利要求1所述的一种提高钛锡酸钡在还原气氛下介电性能的方法，其特征在于，所述步骤(2)的粉料与氧化锆球、去离子水的质量比为1∶1∶2。
4.根据权利要求1所述的一种提高钛锡酸钡在还原气氛下介电性能的方法，其特征在于，所述步骤(5)的坯体为Φ10mm×1mm的圆片。
5.根据权利要求1所述的一种提高钛锡酸钡在还原气氛下介电性能的方法，其特征在于，所述步骤(5)的烧结温度为1400℃。
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