CN107522486A - 一种高调谐率锆钛酸钡陶瓷的制备方法 - Google Patents

一种高调谐率锆钛酸钡陶瓷的制备方法 Download PDF

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CN107522486A
CN107522486A CN201710859986.1A CN201710859986A CN107522486A CN 107522486 A CN107522486 A CN 107522486A CN 201710859986 A CN201710859986 A CN 201710859986A CN 107522486 A CN107522486 A CN 107522486A
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tuning rate
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barium zirconium
ceramics
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李玲霞
郑浩然
于仕辉
陈思亮
孙正
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Tianjin University
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    • C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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Abstract

本发明公开了一种高调谐率锆钛酸钡陶瓷的制备方法，先将BaCO3、ZrO2和TiO2三种原料按照BaZr0.2Ti0.8O3的化学计量比进行混合配料，经过一次球磨后于900～1100℃预烧，形成BZT主晶向，再经二次球磨、烘干、过筛后压制成型为陶瓷生坯，再经排胶后于1200‑1400℃烧结，制得高调谐率锆钛酸钡陶瓷。本发明的锆钛酸钡陶瓷调谐率≥60％，制备成本低，工艺流程简单，具有良好的应用前景。

Description

一种高调谐率锆钛酸钡陶瓷的制备方法
技术领域
本发明是关于电子信息材料与元器件的，具体涉及一种高调谐率锆钛酸钡陶瓷的制备方法。
背景技术
近年来，由于微波移动通信的发展需求，对以微波介质陶瓷为基础的微波电路提出了更高的要求。各种微波控制电路实现对微波信号频率、相位、幅度等的控制功能，是相控阵雷达、多波束雷达、电子对抗技术、微波通讯和微波测量技术的关键技术，压控微波器件是微波控制电路的关键元器件。与不可调器件相比，可调微波器件可工作在不同的频率，增加了电路的实用性和功能性，并且减少了电路尺寸和成本。微波介质陶瓷在可调谐振器、移相器和变容管等微波器件拥有广阔的应用前景，其作为微波电路极佳的电介质材料迅速地发展起来。
钙钛矿锆钛酸钡(BaZrxTi1-xO3，BZT)陶瓷具有优异的介电调谐特性。研究表明，顺电相介电调谐特性可认为是外加电场使铁电体的软模频率升高的结果。并且软模对外加电场硬化的敏感性决定介电调谐量，越接近居里温度，敏感性越强，介电调谐特性越强。在BZT材料中，随Zr含量的增加，居里温度降低，当Zr/Ti比为0.2/0.8时，居里温度在室温附近，根据材料应用环境需求，选择BaZr0.2Ti0.8O3组分陶瓷。
发明内容
本发明的目的，在于克服现有陶瓷对外加电场敏感程度的不足，提供一种高调谐率锆钛酸钡陶瓷的制备方法。
本法明通过如下技术方案予以实现。
一种高调谐率锆钛酸钡陶瓷的制备方法，具体步骤如下：
(1)配料
将BaCO3、ZrO2和TiO2三种原料按照BaZr0.2Ti0.8O3的化学计量比进行混合配料；
(2)一次球磨
将步骤(1)的混合原料，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，将粉料烘干，再进行预烧，形成BZT主晶向，预烧温度为900～1100℃，保温时间为2～4小时；
(4)二次球磨
预烧完成后，外加0.5～1wt％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，将粉料烘干，过40～200目筛；
(6)压制成型
将过筛之后的粉料放入模具中，压制成型为陶瓷生坯；
(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
排胶完成后于1200-1400℃进行烧结，保温时间为3-6小时，制得高调谐率锆钛酸钡陶瓷。
所述步骤(1)的BaCO3、ZrO2和TiO2原料质量纯度在99％以上。
所述步骤(2)或(4)的原料与去离子水和氧化锆磨球的体积比为1:1:1。
所述步骤(3)的预烧温度为1000℃。
所述步骤(7)的排胶温度为700℃。
所述步骤(8)的烧结温度为1350℃。
本发明的锆钛酸钡陶瓷调谐率≥60％，制备成本低，工艺流程简单，具有良好的应用前景。
附图说明
图1为实施例1的锆钛酸钡陶瓷制品的介电性能(电场可调)图谱。
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)选取原料为质量纯度在99％以上的BaCO3、ZrO2和TiO2，按照BaZr0.2Ti0.8O3的化学计量比进行混合。
(2)将上述混合后的原料，加入去离子水和氧化锆磨球，球磨6小时，原料、去离子水与磨球的体积比为1:1:1。
(3)一次球磨完成后，将粉料烘干，之后放入中温马弗炉中进行预烧，预烧温度为1000℃，保温时间为3小时。
(4)预烧完成后，加入0.75wt％PVA，加入去离子水和氧化锆磨球，球磨时为12小时，粉料、去离子水与磨球的体积比约为1:1:1。
(5)二次球磨完成后，将粉料于100℃烘干，过80目筛。
(6)将过筛之后的粉料放入模具中，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)将排胶完成后的坯体进行烧结，烧结温度为1350℃，保温时间为4小时。
所制得的锆钛酸钡陶瓷制品的介电性能：(电场可调)调谐率为76％。
图1为实施例1的锆钛酸钡陶瓷制品的介电性能(电场可调)图谱。由图1可以看出，在600V电压下，锆钛酸钡陶瓷制品的调谐率为76％。
实施例2
(1)选取原料为纯度在99％以上的BaCO3、ZrO2和TiO2，按照BaZr0.2Ti0.8O3的化学计量比进行混合。
(2)将上述混合后的原料，加入去离子水和氧化锆磨球，球磨为6小时，原料、去离子水和磨球的体积比为1:1:1。
(3)一次球磨完成后，将粉料烘干，之后放入中温马弗炉中进行预烧，预烧温度为1000℃，保温时间为3小时。
(4)预烧完成后，加入0.75wt％PVA，加入去离子水和氧化锆磨球，球磨12小时，粉料、去离子水和磨球的体积比为1:1:1。
(5)二次球磨完成，将粉料于100℃烘干，过80目筛。
(6)将过筛之后的粉料放入模具中，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)将排胶完成后的坯体进行烧结，烧结温度为1375℃，保温时间为4小时。
所制得的锆钛酸钡陶瓷制品的介电性能：(电场可调)调谐率为64％。

Claims (6)

1.一种高调谐率锆钛酸钡陶瓷的制备方法，具体步骤如下：
(1)配料
将BaCO3、ZrO2和TiO2三种原料按照BaZr0.2Ti0.8O3的化学计量比进行混合配料；
(2)一次球磨
将步骤(1)的混合原料，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，将粉料烘干，再进行预烧，形成BZT主晶向，预烧温度为900～1100℃，保温时间为2～4小时；
(4)二次球磨
预烧完成后，外加0.5～1wt％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，将粉料烘干，过40～200目筛；
(6)压制成型
将过筛之后的粉料放入模具中，压制成型为陶瓷生坯；
(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
排胶完成后于1200-1400℃进行烧结，保温时间为3-6小时，制得高调谐率锆钛酸钡陶瓷。
2.根据权利要求1所述的一种高调谐率锆钛酸钡陶瓷的制备方法，其特征在于，所述步骤(1)的BaCO3、ZrO2和TiO2原料质量纯度在99％以上。
3.根据权利要求1所述的一种高调谐率锆钛酸钡陶瓷的制备方法，其特征在于，所述步骤(2)或(4)的原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所述的一种高调谐率锆钛酸钡陶瓷的制备方法，其特征在于，所述步骤(3)的预烧温度为1000℃。
5.根据权利要求1所述的一种高调谐率锆钛酸钡陶瓷的制备方法，其特征在于，所述步骤(7)的排胶温度为700℃。
6.根据权利要求1所述的一种高调谐率锆钛酸钡陶瓷的制备方法，其特征在于，所述步骤(8)的烧结温度为1350℃。
CN201710859986.1A 2017-09-21 2017-09-21 一种高调谐率锆钛酸钡陶瓷的制备方法 Pending CN107522486A (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318817A (zh) * 2008-06-25 2008-12-10 重庆科技学院 制备锆钛酸钡陶瓷材料的方法
CN103387390A (zh) * 2013-06-26 2013-11-13 天津大学 改善锆钛酸钡介电陶瓷材料直流偏场可调性的方法
CN107056292A (zh) * 2017-04-26 2017-08-18 天津大学 一种具有低介电损耗的锆钛酸钡陶瓷材料及其制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318817A (zh) * 2008-06-25 2008-12-10 重庆科技学院 制备锆钛酸钡陶瓷材料的方法
CN103387390A (zh) * 2013-06-26 2013-11-13 天津大学 改善锆钛酸钡介电陶瓷材料直流偏场可调性的方法
CN107056292A (zh) * 2017-04-26 2017-08-18 天津大学 一种具有低介电损耗的锆钛酸钡陶瓷材料及其制备方法

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