CN106966721A - 一种具有高介电常数的锆钛酸钡陶瓷材料及其制备方法 - Google Patents

一种具有高介电常数的锆钛酸钡陶瓷材料及其制备方法 Download PDF

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CN106966721A
CN106966721A CN201710281726.0A CN201710281726A CN106966721A CN 106966721 A CN106966721 A CN 106966721A CN 201710281726 A CN201710281726 A CN 201710281726A CN 106966721 A CN106966721 A CN 106966721A
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zirconium titanate
titanate ceramic
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李玲霞
孙正
杜明昆
卢特
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Tianjin University
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Abstract

本发明公开了一种具有高介电常数的锆钛酸钡陶瓷材料及其制备方法，其化学式为：Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/3Nb4/3O7，x＝0.02～0.5。分别将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，为粉料1；再将Bi2O3、ZnO、Nb2O5化学计量式Bi2Zn2/3Nb4/3O7进行配料，为粉料2；将粉料1和粉料2分别球磨、烘干、过筛后分别于600～800℃和1050～1200℃预烧，再将粉料1与粉料2按照化学式Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/3Nb4/3O7，x＝0.02～0.5进行混合，再经球磨、烘干、过筛后，压制成型为坯体，坯体于1275℃～1350℃烧结，制成具有高介电常数的锆钛酸钡陶瓷材料。本发明介电常数εr为5000～30000，介电损耗为0.006～0.2，可适应电子器件不断向集成化和低损耗方向发展的需要。

Description

一种具有高介电常数的锆钛酸钡陶瓷材料及其制备方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，尤其涉及一种具有高介电常数的Ba(Zr0.2Ti0.8)O3(锆钛酸钡)陶瓷材料及其制备方法。
背景技术
随着下一代电子装备逐渐向小型化、信息化和高智能化方向的发展，对电子器件也提出了微型化、集成化、低能耗的要求。陶瓷电容器是电子装备中使用数量较多的电子元器件，减小电容器的尺寸对于实现电子器件和电子装备的小型化至关重要。
锆钛酸钡(Ba(Zr0.2Ti0.8)O3)是BaZrO3掺杂BaTiO3所形成固溶体系。该体系具有高的介电常数(～20000)和适中的介电损耗(～0.08)，为了适应电子器件小型向小型化方向的发展，需要进一步提高锆钛酸钡陶瓷材料的介电常数并进一步降低损耗。
发明内容
本发明的目的，是为提高Ba(Zr0.2Ti0.8)O3陶瓷材料的介电常数，以适应电子器件不断向集成化和低损耗方向发展的需要，主要以BaCO3、TiO2、ZrO2、Bi2O3、ZnO、Nb2O5为原料，通过固相法制备一种具有高介电常数的锆钛酸钡陶瓷材料。
本发明通过如下技术方案予以实现。
一种具有高介电常数的锆钛酸钡陶瓷材料，其化学式为：Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/3Nb4/3O7，x＝0.02～0.5；
该锆钛酸钡陶瓷材料的制备方法，具体如下步骤：
(1)分别将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，称为粉料1；将Bi2O3、ZnO、Nb2O5化学计量式Bi2Zn2/3Nb4/3O7进行配料，称为粉料2，将粉料1和粉料2分别放入球磨罐中，加入去离子水和锆球后，分别球磨2～6小时和4～8小时；
(2)将步骤(1)球磨后的粉料1和粉料2放入干燥箱中，于100～120℃烘干，然后过40目筛；
(3)将过筛后的粉料1和粉料2放入中温炉中，分别于600～800℃和1050～1200℃预烧，保温2～6小时；
(4)将步骤(3)预烧后的粉料1与粉料2按照化学式Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/ 3Nb4/3O7，x＝0.02～0.5进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨10～15小时，烘干后过筛，再用粉末压片机以2～6MPa的压力压制成坯体；
(5)将步骤(4)的坯体于1275℃～1350℃烧结，保温2～8小时，制成具有高介电常数的锆钛酸钡陶瓷材料。
所述步骤(1)的粉料1和粉料2采用行星式球磨机进行球磨，球磨机转速为400转/分。
所述步骤(4)的坯体直径为10mm，厚度为1mm。
所述步骤(5)的烧结温度为1300℃。
所述步骤(4)Bi2Zn2/3Nb4/3O7的掺杂比例为0.2mol％。
本发明通过固相法提供了一种具有高介电常数的锆钛酸钡陶瓷材料Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/3Nb4/3O7，x＝0.02～0.5。其介电常数εr为5000～30000，介电损耗为0.006～0.2，可适应电子器件不断向集成化和低损耗方向发展的需要。
具体实施方式
本发明以BaCO3(分析纯)、TiO2(分析纯)、ZrO2(分析纯)、Bi2O3(分析纯)、ZnO(分析纯)、Nb2O5(分析纯)为初始原料，通过简单固相法制备陶瓷电容器用介质材料。
具体实施例如下：
实施例1
(1)将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，配比为：16.4797gBaCO3、5.3375g TiO2、2.058g ZrO2，将约20g的混合粉料放入尼龙罐中，加入200ml去离子水，加入150g的锆球后，在行星式球磨机上球磨6小时，转速为400转/分；将Bi2O3、ZnO、Nb2O5按照化学计量式Bi2Zn2/3Nb4/3O7进行配料，配比为：8.4719g，1.4801g，3.19g，将约10g的混合粉料放入尼龙罐中，加入200ml去离子水，加入150g的锆球后，在行星式球磨机上球磨4小时，转速为400转/分
(2)将球磨后的粉料1和粉料2分别置于干燥箱中，于100℃烘干，之后过40目筛；
(3)将过筛后的粉料1放入中温炉，于750℃预烧，保温4小时；再将粉料2放入中温炉，于1100℃预烧，保温4小时
(4)将步骤(3)预烧后的粉料1和粉料2按化学计量式Ba(Zr0.2Ti0.8)O3+0.2mol％Bi2Zn2/3Nb4/3O7进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨12小时，烘干后过筛，再用粉末压片机以4MPa的压力压制成坯体；
(5)将坯体在1300℃烧结，保温4小时，制成具有高介电常数的锆钛酸钡陶瓷材料。
(6)通过HEWLETT PACKARD 4278A测试其在室温，1kHz下的介电性能，其性能如下：
介电常数为：29551
介电损耗为：0.04
实施例2～5
实施例2～5的制备过程与实施例1基本相同，主要区别在于Bi2Zn2/3Nb4/3O7含量的不同；具体实施例的工艺参数与其相关的介电性能详见表1
表1

Claims (5)

1.一种具有高介电常数的锆钛酸钡陶瓷材料，其化学式为：Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/3Nb4/3O7，x＝0.02～0.5。
该锆钛酸钡陶瓷材料的制备方法，具体如下步骤：
(1)分别将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，称为粉料1；将Bi2O3、ZnO、Nb2O5化学计量式Bi2Zn2/3Nb4/3O7进行配料，称为粉料2，将粉料1和粉料2分别放入球磨罐中，加入去离子水和锆球后，分别球磨2～6小时和4～8小时；
(2)将步骤(1)球磨后的粉料1和粉料2放入干燥箱中，于100～120℃烘干，然后过40目筛；
(3)将过筛后的粉料1和粉料2放入中温炉中，分别于600～800℃和1050～1200℃预烧，保温2～6小时；
(4)将步骤(3)预烧后的粉料1与粉料2按照化学式Ba(Zr0.2Ti0.8)O3+xmol％Bi2Zn2/3Nb4/ 3O7，x＝0.02～0.5进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨10～15小时，烘干后过筛，再用粉末压片机以2～6MPa的压力压制成坯体；
(5)将步骤(4)的坯体于1275℃～1350℃烧结，保温2～8小时，制成具有高介电常数的锆钛酸钡陶瓷材料。
2.根据权利要求1所述的一种具有高介电常数的锆钛酸钡陶瓷材料，其特征在于，所述步骤(1)的粉料1和粉料2采用行星式球磨机进行球磨，球磨机转速为400转/分。
3.根据权利要求1所述的一种具有高介电常数的锆钛酸钡陶瓷材料，其特征在于，所述步骤(4)的坯体直径为10mm，厚度为1mm。
4.根据权利要求1所述的一种具有高介电常数的锆钛酸钡陶瓷材料，其特征在于，所述步骤(5)的烧结温度为1300℃。
5.根据权利要求1所述的一种具有高介电常数的锆钛酸钡陶瓷材料，其特征在于，所述步骤(4)Bi2Zn2/3Nb4/3O7的掺杂比例为0.2mol％。
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