CN108610040A - 一种降低钛锡酸钡体系在还原气氛下介电损耗的方法 - Google Patents

一种降低钛锡酸钡体系在还原气氛下介电损耗的方法 Download PDF

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CN108610040A
CN108610040A CN201810393110.7A CN201810393110A CN108610040A CN 108610040 A CN108610040 A CN 108610040A CN 201810393110 A CN201810393110 A CN 201810393110A CN 108610040 A CN108610040 A CN 108610040A
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李玲霞
王瑞杰
张宁
于仕辉
孙正
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Abstract

本发明公开了一种降低钛锡酸钡在还原气氛下介电损耗的方法，先将原料BaTiO3、SnO2、BaCO3按Ba(SnxTi1‑x)O3，其中0＜x≤0.3化学式称量配料，经球磨、烘干、过筛后于1050℃下煅烧，合成主晶相；再经二次球磨后外加粘结剂进行造粒；再将造粒粉料压制成生坯，生坯排胶后，在还原气氛下于1350～1450℃烧结，制得在还原气氛下低损耗钛锡酸钡介质材料。本发明通过增加二次球磨工艺，其介电损耗由现有技术的1.0％～5.0％降至0.5％～4.0％，从而大大提高了多层片式陶瓷电容器的性能。

Description

一种降低钛锡酸钡体系在还原气氛下介电损耗的方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种降低钛锡酸钡介电损耗的方法。
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***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，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。在实现介质材料的抗还原的基础上，需要对介质材料的介电性能进行优化。介电损耗为是指在单位时间内每单位体积中将电能转化为热能而消耗的能量。这一部分的能量消耗降低了MLCC的转化效率，因此降低介电损耗有益于增加介质材料的使用效率。
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，是在钛锡酸钡还原气氛下烧结的工艺条件下，提供一种提高其介电性能、降低介电损耗的方法。
本发明通过如下技术方案予以实现。
一种降低钛锡酸钡在还原气氛下介电损耗的方法，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；再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1050℃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，二次球磨，加入氧化锆球和去离子水，球磨4小时；再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1350～1450℃烧结，保温2～4小时，制得在还原气氛下低损耗钛锡酸钡的介质材料。
所述步骤(2)、(4)的烘干温度为100℃。
所述步骤(2)、(4)的粉料与氧化锆球、去离子水的质量比为1∶1∶2。
所述步骤(6)的坯体为Φ10mm×1mm的圆片。
所述步骤(6)的烧结温度为1400℃。
所述步骤(6)的还原气氛为H2:N2＝1:20。
本发明提供了一种降低钛锡酸钡在还原气氛下介电损耗的方法，通过增加二次球磨工艺，制得的Ba(SnxTi1-x)O3介质材料的介电损耗由现有技术的1.0％～5.0％降至0.5％～4.0％。由于介电损耗的降低，大大提高了多层片式陶瓷电容器的性能。
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(Sn0.05Ti0.95)O3化学式称量配料；
(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)合成主晶相的粉料放入球磨罐中，二次球磨，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)处理后的的粉料外加质量百分比为7％的粘结剂，过80目分样筛，造粒；
(6)将步骤(5)的造粒粉料用粉末压片机以6MPa的压力压成Φ10mm×1mm的坯体，经排胶后，在H2:N2＝1:20的还原气氛比例下，于1350℃烧结，保温3小时，制得在还原气氛下高介电常数低损耗低频钛锡酸钡介质材料；
(7)采用TH2828S测试其样品的介电损耗，1KHz下，tanδ＝3.7％。
实施例2～8
实施例2～8的主要工艺参数及其介质损耗详见表1，其余制备工艺与实施例1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 (6)

1.一种降低钛锡酸钡在还原气氛下介电损耗的方法，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；再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1050℃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，二次球磨，加入氧化锆球和去离子水，球磨4小时；再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1350～1450℃烧结，保温2～4小时，制得在还原气氛下低损耗钛锡酸钡介质材料。
2.根据权利要求1所述的一种降低钛锡酸钡体系在还原气氛下介电损耗的方法，其特征在于，所述步骤(2)、(4)的烘干温度为100℃。
3.根据权利要求1所述的一种降低钛锡酸钡体系在还原气氛下介电损耗的方法，其特征在于，所述步骤(2)、(4)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所述的一种降低钛锡酸钡体系在还原气氛下介电损耗的方法，其特征在于，所述步骤(6)的坯体为Φ10mm×1mm的圆片。
5.根据权利要求1所述的一种降低钛锡酸钡体系在还原气氛下介电损耗的方法，其特征在于，所述步骤(6)的烧结温度为1400℃。
6.根据权利要求1所述的一种降低钛锡酸钡体系在还原气氛下介电损耗的方法，其特征在于，所述步骤(6)的还原气氛为H2:N2＝1:20。
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