CN109231983A - 一种双层锆钛酸钡基陶瓷的制备方法 - Google Patents

一种双层锆钛酸钡基陶瓷的制备方法 Download PDF

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CN109231983A
CN109231983A CN201811216127.1A CN201811216127A CN109231983A CN 109231983 A CN109231983 A CN 109231983A CN 201811216127 A CN201811216127 A CN 201811216127A CN 109231983 A CN109231983 A CN 109231983A
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ion doping
barium
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李玲霞
郑浩然
于仕辉
杨盼
彭伟
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Abstract

本发明公开了一种双层锆钛酸钡基陶瓷的制备方法，先将BaCO3、ZrO2、TiO2和Nb2O5，按照BaZr0.2Ti0.8O3+0.2mol％Nb2O5的化学计量比制备Nb5+离子掺杂锆钛酸钡原料；再将BaCO3、Bi2O3、ZrO2和TiO2按照Ba0.9988Bi0.0008Zr0.2Ti0.8O3的化学计量比制备Bi3+离子掺杂锆钛酸钡的原料；再分别经过一次球磨、预烧、二次球磨、过筛；再先将Nb5+离子掺杂锆钛酸钡粉料放入模具中并抚平，然后再将Bi3+离子掺杂锆钛酸钡粉料放入模具中并抚平，压制成型为陶瓷生坯，Nb5+离子掺杂与Bi3+离子掺杂粉料的质量比为1:0.5～1:2；坯体经过排胶后1200～1300℃烧结，制得双层锆钛酸钡基陶瓷。本发明介电常数＞15000@1kHz，介电损耗＜0.2@1kHz，工艺流程简单，具有良好的应用前景。

Description

一种双层锆钛酸钡基陶瓷的制备方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，具体涉及一种双层锆钛酸钡基陶瓷的制备方法。
背景技术
在电子工业领域，陶瓷电容器具有举足轻重的地位，其在耐高温、耐腐蚀、抗辐射等方面具有很大优势，并且介电常数较高，广泛应用于通讯设备、家用电器、仪器仪表、武器装备等军事和民用领域。随着集成电路的快速发展，陶瓷电容器朝着小型化、大容量、低损耗方向发展，铅基钙钛矿结构介质材料具有良好的介电性能，但其含有易挥发、毒性的铅元素，为走可持续发展道路，各国逐步实施了电子陶瓷的无铅化管制。
无铅锆钛酸钡基陶瓷材料是Zr4+离子部分取代钛酸钡中Ti4+离子后形成的固溶体，随着Zr4+离子含量的变化，居里温度向室温方向移动，同时伴随介电性能的改善。研究表明Nb5+离子掺杂取代Ti4+离子，其作为施主掺杂，当添加量较低时补偿机制为自由电子补偿，造成材料内部半导化，介电常数增大，但同时带来介电损耗的升高。为兼具较高介电常数和较低介电损耗，采用低损耗的Bi3+离子掺杂锆钛酸钡材料与高介电常数的Nb5+离子掺杂锆钛酸钡材料复合，制成一种双层陶瓷结构，将两者的优势进行融合。
发明内容
本发明的目的，在现有技术的基础上，为兼具较高介电常数和较低介电损耗，采用低损耗的Bi3+离子掺杂锆钛酸钡材料与高介电常数的Nb5+离子掺杂锆钛酸钡材料复合，将两者的优势进行融合，提供一种双层锆钛酸钡基陶瓷的制备方法。
本发明通过如下技术方案予以实现。
一种双层锆钛酸钡基陶瓷的制备方法，具体步骤如下：
(1)配料
制备Nb5+离子掺杂锆钛酸钡的原料为BaCO3、ZrO2、TiO2和Nb2O5，四种原料按照BaZr0.2Ti0.8O3+0.2mol％Nb2O5的化学计量比进行混合配料；
制备Bi3+离子掺杂锆钛酸钡的原料为BaCO3、Bi2O3、ZrO2和TiO2，四种原料按照Ba0.9988Bi0.0008Zr0.2Ti0.8O3的化学计量比进行混合配料；
(2)一次球磨
将步骤(1)的两种陶瓷粉料分别进行一次球磨，加入去离子水和氧化锆磨球，球磨4～8小时，使粉料细化；
(3)预烧
一次球磨完成后，待粉料烘干，将两种陶瓷粉料分别进行预烧，预烧温度为1000～1200℃，保温时间为3～5小时；
(4)二次球磨
预烧完成后，将两种陶瓷粉料分别外加0.25～0.75wt％的塑化剂PVA，加入去离子水和氧化锆磨球，进行二次球磨，球磨10～14小时；
(5)过筛
二次球磨完成后，待粉料烘干，将两种陶瓷粉料分别过40～200目筛；
(6)压制成型
首先将过筛之后的Nb5+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，然后再将过筛之后的Bi3+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，压制成型为陶瓷生坯，Nb5 +离子掺杂与Bi3+离子掺杂的锆钛酸钡粉料的质量比为1:0.5～1:2；
(7)排胶
将压制成型后的陶瓷生坯放入低温炉中进行排胶，排胶温度600-800℃；
(8)烧结
将排胶完成后的坯体于1200～1300℃进行烧结，保温时间为3～6小时，制得双层锆钛酸钡基陶瓷。
所述步骤(1)的BaCO3、ZrO2、TiO2、Nb2O5和Bi2O3原料质量纯度在99％以上。
所述步骤(2)或(4)的粉料与去离子水和氧化锆磨球的体积比为1:1:1。
所述步骤(8)的烧结温度为1260℃。
本发明公开的双层锆钛酸钡基陶瓷介电常数高(＞15000@1kHz)，介电损耗低(＜0.2@1kHz)，工艺流程简单，具有良好的应用前景。
具体实施方式
下面结合具体实施例进一步阐述本发明，应理解，这些实施例仅用于说明本发明而不用于限制本发明的保护范围。
实施例1
(1)制备Nb5+离子掺杂锆钛酸钡的原料为纯度在99％以上的BaCO3、ZrO2、TiO2和Nb2O5，四种原料按照BaZr0.2Ti0.8O3+0.2mol％Nb2O5的比例进行混合配料；制备Bi3+离子掺杂锆钛酸钡的原料为纯度在99％以上的BaCO3、Bi2O3、ZrO2和TiO2，四种原料按照Ba0.9988Bi0.0008Zr0.2Ti0.8O3的化学计量比进行混合配料。
(2)将步骤(1)的两种陶瓷粉料分别进行一次球磨，加入去离子水和氧化锆磨球，粉料、去离子水和磨球的体积比为1:1:1，球磨时间为6小时。
(3)一次球磨完成后，待粉料烘干，将两种陶瓷粉料分别进行预烧，预烧温度为1100℃，保温时间为4小时。
(4)预烧完成后，将两种陶瓷粉料分别加入0.5wt％的PVA，加入去离子水和氧化锆磨球，进行二次球磨，粉料、去离子水和磨球的体积比为1:1:1，球磨时间为12小时。
(5)二次球磨完成，待粉料烘干，将两种陶瓷粉料分别过80目筛。
(6)首先将0.2克过筛之后的Nb5+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，然后将0.1克过筛之后的Bi3+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，压制成型为陶瓷生坯。
(7)压制成型后的陶瓷生坯放入低温炉中进行排胶，排胶温度700℃。
(8)排胶完成后进行烧结，烧结温度为1300℃，保温时间为4小时。
所制得的双层锆钛酸钡基陶瓷介电常数为32800@1kHz，介电损耗为0.18@1kHz。
实施例2
(1)制备Nb5+离子掺杂锆钛酸钡的原料为纯度在99％以上的BaCO3、ZrO2、TiO2和Nb2O5，四种原料按照BaZr0.2Ti0.8O3+0.2mol％Nb2O5的比例进行混合配料；制备Bi3+离子掺杂锆钛酸钡的原料为纯度在99％以上的BaCO3、Bi2O3、ZrO2和TiO2，四种原料按照Ba0.9988Bi0.0008Zr0.2Ti0.8O3的化学计量比进行混合配料。
(2)将步骤(1)的两种陶瓷粉料分别进行一次球磨，加入去离子水和氧化锆磨球，粉料、去离子水和磨球的体积比为1:1:1，球磨时间为6小时。
(3)一次球磨完成后，待粉料烘干，将两种陶瓷粉料分别进行预烧，预烧温度为1100℃，保温时间为4小时。
(4)预烧完成后，将两种陶瓷粉料分别加入0.5wt％的PVA，加入去离子水和氧化锆磨球，进行二次球磨，粉料、去离子水和磨球的体积比为1:1:1，球磨时间为12小时。
(5)二次球磨完成，待粉料烘干，将两种陶瓷粉料分别过80目筛。
(6)首先将0.15克过筛之后的Nb5+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，然后将0.15克过筛之后的Bi3+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，压制成型为陶瓷生坯。
(7)压制成型后的陶瓷生坯放入低温炉中进行排胶，排胶温度700℃。
(8)排胶完成后进行烧结，烧结温度为1260℃，保温时间为4小时。
所制得的双层锆钛酸钡基陶瓷介电常数为23400@1kHz，介电损耗为0.15@1kHz。
实施例3
(1)制备Nb5+离子掺杂锆钛酸钡的原料为纯度在99％以上的BaCO3、ZrO2、TiO2和Nb2O5，四种原料按照BaZr0.2Ti0.8O3+0.2mol％Nb2O5的比例进行混合配料；制备Bi3+离子掺杂锆钛酸钡的原料为纯度在99％以上的BaCO3、Bi2O3、ZrO2和TiO2，四种原料按照Ba0.9988Bi0.0008Zr0.2Ti0.8O3的化学计量比进行混合配料。
(2)将步骤(1)的两种陶瓷粉料分别进行一次球磨，加入去离子水和氧化锆磨球，粉料、去离子水和磨球的体积比为1:1:1，球磨时间为6小时。
(3)一次球磨完成后，待粉料烘干，将两种陶瓷粉料分别进行预烧，预烧温度为1100℃，保温时间为4小时。
(4)预烧完成后，将两种陶瓷粉料分别加入0.5wt％的PVA，加入去离子水和氧化锆磨球，进行二次球磨，粉料、去离子水和磨球的体积比为1:1:1，球磨时间为12小时。
(5)二次球磨完成，待粉料烘干，将两种陶瓷粉料分别过80目筛。
(6)首先将0.1克过筛之后的Nb5+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，然后将0.2克过筛之后的Bi3+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，压制成型为陶瓷生坯。
(7)压制成型后的陶瓷生坯放入低温炉中进行排胶，排胶温度700℃。
(8)排胶完成后进行烧结，烧结温度为1200℃，保温时间为4小时。
所制得的双层锆钛酸钡基陶瓷介电常数为15300@1kHz，介电损耗为0.06@1kHz。

Claims (4)

1.一种双层锆钛酸钡基陶瓷的制备方法，具体步骤如下：
(1)配料
制备Nb5+离子掺杂锆钛酸钡的原料为BaCO3、ZrO2、TiO2和Nb2O5，四种原料按照BaZr0.2Ti0.8O3+0.2mol％Nb2O5的化学计量比进行混合配料；
制备Bi3+离子掺杂锆钛酸钡的原料为BaCO3、Bi2O3、ZrO2和TiO2，四种原料按照Ba0.9988Bi0.0008Zr0.2Ti0.8O3的化学计量比进行混合配料；
(2)一次球磨
将步骤(1)的两种陶瓷粉料分别进行一次球磨，加入去离子水和氧化锆磨球，球磨4～8小时，使粉料细化；
(3)预烧
一次球磨完成后，待粉料烘干，将两种陶瓷粉料分别进行预烧，预烧温度为1000～1200℃，保温时间为3～5小时；
(4)二次球磨
预烧完成后，将两种陶瓷粉料分别外加0.25～0.75wt％的塑化剂PVA，加入去离子水和氧化锆磨球，进行二次球磨，球磨10～14小时；
(5)过筛
二次球磨完成后，待粉料烘干，将两种陶瓷粉料分别过40～200目筛；
(6)压制成型
首先将过筛之后的Nb5+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，然后再将过筛之后的Bi3+离子掺杂锆钛酸钡粉料放入模具中，将粉料抚平，压制成型为陶瓷生坯，Nb5+离子掺杂与Bi3+离子掺杂的锆钛酸钡粉料的质量比为1:0.5～1:2；
(7)排胶
将压制成型后的陶瓷生坯放入低温炉中进行排胶，排胶温度600-800℃；
(8)烧结
将排胶完成后的坯体于1200～1300℃进行烧结，保温时间为3～6小时，制得双层锆钛酸钡基陶瓷。
2.根据权利要求1所述的一种双层锆钛酸钡基陶瓷的制备方法，其特征在于，所述步骤(1)的BaCO3、ZrO2、TiO2、Nb2O5和Bi2O3原料质量纯度在99％以上。
3.根据权利要求1所述的一种双层锆钛酸钡基陶瓷的制备方法，其特征在于，所述步骤(2)或(4)的粉料与去离子水和氧化锆磨球的体积比为1:1:1。
4.根据权利要求1所述的一种双层锆钛酸钡基陶瓷的制备方法，其特征在于，所述步骤(8)的烧结温度为1260℃。
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