CN104310986B - 一种高介电常数温度稳定型陶瓷电容器介质材料 - Google Patents

一种高介电常数温度稳定型陶瓷电容器介质材料 Download PDF

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CN104310986B
CN104310986B CN201410525530.8A CN201410525530A CN104310986B CN 104310986 B CN104310986 B CN 104310986B CN 201410525530 A CN201410525530 A CN 201410525530A CN 104310986 B CN104310986 B CN 104310986B
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ceramic capacitor
dielectric material
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李玲霞
金雨馨
董和磊
于仕辉
许丹
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Abstract

本发明公开了一种高介电常数温度稳定型陶瓷电容器介质材料，化学式为(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7；先将原料Bi2O3、Nb2O5、MnCO3、ZnO按上述化学式称量配料，经球磨、烘干、过筛、煅烧，合成主晶相；再外加质量百分比为0.75％的聚乙烯醇，经球磨、烘干、过筛、压成坯体；坯体于950～1000℃烧结，制成高介电常数温度稳定型陶瓷电容器介质材料。本发明具有较低的烧结温度(950～1000℃)，高的介电常数(129～140)，近零的电容量温度系数(‑29×10‑6/℃～‑18×10‑6/℃)，可用于多层片式陶瓷电容器(MLCC)的制备，由于具有较低的烧结温度，大大降低了器件的成本。

Description

一种高介电常数温度稳定型陶瓷电容器介质材料
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种高介电常数温度稳定型陶瓷电容器介质材料及制备方法。
背景技术
近年来，随着电子线路日益微型化、集成化和高频化，电子元件必须尺寸小，具有高频、高可靠、价格低廉和高集成度等特性。铋基焦绿石介质材料作为一类新兴的低温烧结陶瓷材料，其介电常数高，介质损耗小，烧结温度低，介电常数温度系数可调且不含Pb，被广泛应用于高频器件中。
立方焦绿石Bi1.5ZnNb1.5O7系陶瓷是以Bi2O3-ZnO-Nb2O5三元系统为基础的陶瓷介质，其具有烧结温度低、介电常数高(εr≈150)、介电损耗小等优点，并且其不与Ag内电极浆料起反应，可采用低钯含量的银钯浆料作为内电极，应用于多层片式陶瓷电容器(MLCC)的制备，并大大降低多层器件的成本。然而，材料的电容量温度系数非常低(TCC≈-400×10-6/℃)，不利于实际应用。因此，调节体系的电容量温度系数，提高体系的温度稳定性，同时保持较高的介电常数，成为研究者急需解决的关键问题。
发明内容
本发明的目的，是为克服现有技术制备的陶瓷介质材料介电常数低、温度稳定性差的缺点，提供一种具有高介电常数的温度稳定型陶瓷电容器介质材料及制备方法。
本发明通过如下技术方案予以实现。
一种高介电常数温度稳定型陶瓷电容器介质材料，化学式为(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7；
该高介电常数温度稳定型陶瓷电容器介质材料的制备方法，具有如下步骤：
(1)将原料Bi2O3、Nb2O5、MnCO3、ZnO按(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7化学式称量配料；
(2)将步骤(1)配制的原料放入球磨罐中，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750℃下煅烧4小时，合成主晶相；
(4)在步骤(3)合成主晶相的粉料中外加质量百分比为0.75％的聚乙烯醇，放入球磨罐中，加入氧化锆球和去离子水，球磨12小时，烘干后过80目筛，再用粉末压片机以4MPa的压力压成坯体；
(5)将步骤(4)成型后的坯体于950～1000℃烧结，保温4小时，制成高介电常数温度稳定型陶瓷电容器介质材料；
(6)测试制品的高频介电性能。
所述步骤(2)和步骤(4)的烘干温度为100℃。
所述步骤(2)和步骤(4)的陶瓷粉体与氧化锆球、去离子水的质量比为1∶1∶2。
所述步骤(4)的坯体为Φ10mm×1mm的圆片。
所述步骤(5)烧结温度为975℃。
本发明的有益效果：提供了一种高介电常数温度稳定型陶瓷电容器介质材料及其制备方法，制得的(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7材料，具有较低的烧结温度为950～1000℃，高的介电常数在129～140之间，近零的电容量温度系数在-29×10-6/℃～-18×10-6/℃范围内，可用于多层片式陶瓷电容器(MLCC)的制备，同时材料具有较低的烧结温度，可大大降低多层器件的成本。
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Bi2O3、Nb2O5、MnCO3、ZnO按(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7化学式称量配料；
(2)将上述配制的原料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，原料与氧化锆球、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)将上述混合均匀的粉料于750℃下煅烧4小时，合成主晶相；
(4)在煅烧后合成主晶相的粉料中外加质量百分比为0.75％的聚乙烯醇，放入球磨罐中，加入氧化锆球和去离子水，粉体与氧化锆球、去离子水的质量比为1∶1∶2，球磨12小时，烘干后过80目筛，再用粉末压片机以4MPa的压力压成Φ10mm×1mm的坯体；
(5)将上述成型后的坯体于975℃烧结，保温4小时，制成高介电常数的低温烧结温度稳定型陶瓷电容器介质材料；
(6)采用Agilent4278A阻抗分析仪测试其介电性能，1MHz下，εr＝140,TCC＝-29×10-6/℃。
实施例2
(1)将原料Bi2O3、Nb2O5、MnCO3、ZnO按(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7化学式称量配料；
(2)将上述配制的原料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，原料与氧化锆球、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)将上述混合均匀的粉料于750℃下煅烧4小时，合成主晶相；
(4)在煅烧后合成主晶相的粉料中外加质量百分比为0.75％的聚乙烯醇，放入球磨罐中，加入氧化锆球和去离子水，粉体与氧化锆球、去离子水的质量比为1∶1∶2，球磨12小时，烘干后过80目筛，再用粉末压片机以4MPa的压力压成Φ10mm×1mm的坯体；
(5)将上述成型后的坯体于950℃烧结，保温4小时，制成高介电常数的低温烧结温度稳定型陶瓷电容器介质材料；
(6)采用Agilent4278A阻抗分析仪测试其介电性能，1MHz下，εr＝129,TCC＝-18×10-6/℃。
实施例3
(1)将原料Bi2O3、Nb2O5、MnCO3、ZnO按(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7化学式称量配料；
(2)将上述配制的原料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，原料与氧化锆球、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)将上述混合均匀的粉料于750℃下煅烧4小时，合成主晶相；
(4)在煅烧后合成主晶相的粉料中外加质量百分比为0.75％的聚乙烯醇，放入球磨罐中，加入氧化锆球和去离子水，粉体与氧化锆球、去离子水的质量比为1∶1∶2，球磨12小时，烘干后过80目筛，再用粉末压片机以4MPa的压力压成Φ10mm×1mm的坯体；
(5)将上述成型后的坯体于1000℃烧结，保温4小时，制成高介电常数的低温烧结温度稳定型陶瓷电容器介质材料；
(6)采用Agilent4278A阻抗分析仪测试其介电性能，1MHz下，εr＝133,TCC＝-26×10-6/℃。
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)

1.一种高介电常数温度稳定型陶瓷电容器介质材料，化学式为(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7；
该高介电常数温度稳定型陶瓷电容器介质材料的制备方法，具有如下步骤：
(1)将原料Bi2O3、Nb2O5、MnCO3、ZnO按(Bi1.5Mn0.5)(Zn0.5Nb1.5)O7化学式称量配料；
(2)将步骤(1)配制的原料放入球磨罐中，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750℃下煅烧4小时，合成主晶相；
(4)在步骤(3)合成主晶相的粉料中外加质量百分比为0.75％的聚乙烯醇，放入球磨罐中，加入氧化锆球和去离子水，球磨12小时，烘干后过80目筛，再用粉末压片机以4MPa的压力压成坯体；
(5)将步骤(4)成型后的坯体于950～1000℃烧结，保温4小时，制成高介电常数温度稳定型陶瓷电容器介质材料；
(6)测试制品的高频介电性能。
2.根据权利要求1所述的一种高介电常数温度稳定型陶瓷电容器介质材料，其特征在于，所述步骤(2)和步骤(4)的烘干温度为100℃。
3.根据权利要求1所述的一种高介电常数温度稳定型陶瓷电容器介质材料，其特征在于，所述步骤(2)和步骤(4)的陶瓷粉体与氧化锆球、去离子水的质量比为1∶1∶2。
4.根据权利要求1所述的一种高介电常数温度稳定型陶瓷电容器介质材料，其特征在于，所述步骤(4)的坯体为Φ10mm×1mm的圆片。
5.根据权利要求1所述的一种高介电常数温度稳定型陶瓷电容器介质材料，其特征在于，所述步骤(5)烧结温度为975℃。
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