CN108689703A - 一种具有巨介电常数及电调特性的无铅铁电陶瓷材料及其制备方法 - Google Patents

一种具有巨介电常数及电调特性的无铅铁电陶瓷材料及其制备方法 Download PDF

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CN108689703A
CN108689703A CN201810668019.1A CN201810668019A CN108689703A CN 108689703 A CN108689703 A CN 108689703A CN 201810668019 A CN201810668019 A CN 201810668019A CN 108689703 A CN108689703 A CN 108689703A
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周昌荣
许积文
曾卫东
黎清宁
杨玲
袁昌来
陈国华
饶光辉
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Abstract

本发明公开了一种具有巨介电常数及电调特性的无铅铁电陶瓷材料及其制备方法，该陶瓷材料组成为：(1‑x)BaTi0.90Sn0.10O3‑xCa2LaMn2O7；其中x表示摩尔分数，0.01<x<0.2。其中BaTi0.90Sn0.10O3和Ca2LaMn2O7通过固相合成反应法分开合成，然后通过混合及一次微波烧结形成特殊的小尺度杂化复杂结构，产生巨介电常数及介电常数外场可调特性，这些性能目前超过了所有报道的无铅铁电陶瓷。产品经实验测量，具有巨介电常数及电调特性，介电常数εr~105，介电可调度~98%，性能稳定，成本低廉，适合大规模工业生产。

Description

一种具有巨介电常数及电调特性的无铅铁电陶瓷材料及其制 备方法
技术领域
本发明涉及电容器及电调电容用的无铅铁电陶瓷材料，具体是一种具有巨介电常数及电调特性的无铅铁电陶瓷材料及其制备方法。
背景技术
介电常数是材料相对于真空来说增加电容器电容能力的度量。介电常数随分子偶极矩和可极化性的增大而增大。近十年来，电子元器件的集成化、小型化和高速化是微电子技术发展的主要驱动力，高介电常数材料是电子元器件如动态存储器(Dynamic randomaccess memory，即DRAM)和多层陶瓷电容器(Multilayer ceramic capacitor，即MLCC)的核心材料。巨介电常数陶瓷材料可以进一步突破大容量电容器及电子元件小型化/微型化和高性能发展的“瓶颈”，而受到了广泛关注。
电场可调电介质材料因为在电可调振荡器、电可调滤波器以及移相器等元器件中的重要应用而得到广泛的关注和研究。电场可调电介质材料需要有尽可能高的介电常数电场可调度，同时还要有尽可能低的介电损耗，通常用介电可调性和优值因子(介电可调性损耗)表示。铁电材料介电性能非线性可实现频率和相位捷变，其非线性的实现利用了介电常数外场可调特性，不需要额外附属元件和复杂电路，有利于小型化。
BaTiO3基铁电材料具有大的介电常数及介电常数外场可调特性，但是目前BaTiO3基陶瓷的巨介电特性还很少报道。
发明内容
本发明的目的是提供一种ABO3型钙钛矿结构，具有巨介电常数及介电常数外场可调特性BaTiO3基无铅铁电陶瓷材料及其制备方法，通过钙钛矿结构铁电体BaTi0.90Sn0.10O3和Ruddlesden-Popper结构的Ca2LaMn2O7形成小尺度杂化复杂结构，该陶瓷材料性能稳定，成本低廉。
本发明一种具有巨介电常数及电调特性的无铅铁电陶瓷材料，其组成为：
(1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7； 其中x表示摩尔分数，0.01<x<0.2；
其中BaTi0.90Sn0.10O3和Ca2LaMn2O7通过固相合成法分开合成，然后通过混合及一次微波烧结形成特殊的小尺度杂化复杂结构，产生巨介电常数及介电常数外场可调特性，这些性能目前超过了所有报道的无铅铁电陶瓷。
上述具有巨介电常数及电可调特性的无铅铁电陶瓷材料的制备方法，采用固相合成法，结合微波烧结形成特殊的杂化结构，包括如下步骤：
(1)按照BaTi0.90Sn0.10O3的化学计量分别称取分析纯原料BaCO3、SnO2和TiO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干，再在高铝坩埚中于1200℃保温2小时预合成BaTi0.90Sn0.10O3粉体；
(2)按照Ca2LaMn2O7的化学计量分别称取分析纯原料CaCO3、La2O3和MnO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干, 再在高铝坩埚中于1300℃保温2小时预合成Ca2LaMn2O7粉体；
(3)将合成好的BaTi0.90Sn0.10O3粉体、Ca2LaMn2O7粉体，按照(1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7（其中x表示摩尔分数，0.01<x<0.2）化学计量式配料；
(4)将步骤（3）配料好的原料，以无水乙醇为介质球磨15h，干燥，加入5%的PVA造粒，在150Mpa压力下冷等静压成型；
(5)将步骤（4）成型的原料采用微波快速烧结，在1400℃保温30分钟，烧结成瓷；烧结后的样品加工成两面光滑的薄片，两面镀银电极制备成具有巨介电常数及电调特性的无铅铁电陶瓷材料。
本发明制备的无铅铁电陶瓷材料，经实验测量，介电常数εr~105，介电可调度~98%，具有巨介电常数及介电常数外场可调特性，产品性能稳定，成本低廉，绿色环保，制备方法简单，适合大规模工业生产。
附图说明
图1为实施例无铅铁电陶瓷材料的巨介电常数及介电常数外场可调特性测量图。
具体实施方式
下面结合实施例和附图对本发明内容作进一步的说明，但不是对本发明的限定。
实施例1
一种具有巨介电常数及电可调特性的无铅铁电陶瓷材料，其组成为：(1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7，其中x表示摩尔分数， x=0.02。
上述陶瓷材料的制备方法，具体步骤如下：
(1)按照BaTi0.90Sn0.10O3的化学计量分别称取分析纯原料BaCO3、SnO2和TiO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干, 再在高铝坩埚中于1200℃保温2小时预合成BaTi0.90Sn0.10O3粉体；
(2)按照Ca2LaMn2O7的化学计量分别称取分析纯原料CaCO3、La2O3和MnO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干， 再在高铝坩埚中于1300℃保温2小时预合成Ca2LaMn2O7粉体；
(3)将合成好的BaTi0.90Sn0.10O3粉体、Ca2LaMn2O7粉体，按照(1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7（其中x表示摩尔分数，x=0.02）化学计量式配料；
(4)将步骤（3）配料好的原料，以无水乙醇为介质球磨15h，干燥，加入5%的PVA造粒，在150Mpa冷等静压成型；
(5)将步骤（4）成型的原料采用微波快速烧结，在1400℃保温30分钟，烧结成瓷；烧结后的样品加工成两面光滑的薄片，两面镀银电极制备成具有巨介电常数及电调特性的无铅铁电陶瓷材料。
实施例2
一种具有巨介电常数及电可调特性的无铅铁电陶瓷材料，其组成为：(1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7，其中x表示摩尔分数， x=0.05；
其制备方法同实施例1。
实施例3
一种具有巨介电常数及电可调特性的无铅铁电陶瓷材料，其组成为：(1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7，其中x表示摩尔分数， x=0.12；
其制备方法同实施例1。
实施例1-3制备的陶瓷材料的巨介电常数及介电常数外场可调特性如图1所示。
实施例1-3制备的陶瓷材料，介电性能测量结果，如下表所示：
通过上面给出的实施例，可以进一步清楚的了解本发明的内容，但它们不是对本发明的限定。

Claims (2)

1.一种具有巨介电常数及电调特性的无铅铁电陶瓷材料，其特征在于：该陶瓷材料组成为：(1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7； 其中x表示摩尔分数，0.01<x<0.2。
2.根据权利要求1所述的无铅铁电陶瓷材料的制备方法，其特征在于，包括如下步骤：
（1）按照BaTi0.90Sn0.10O3的化学计量分别称取分析纯原料BaCO3、SnO2和TiO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干，再在高铝坩埚中于1200℃保温2小时预合成BaTi0.90Sn0.10O3粉体；
（2）按照Ca2LaMn2O7的化学计量分别称取分析纯原料CaCO3、La2O3和MnO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干， 再在高铝坩埚中于1300℃保温2小时预合成Ca2LaMn2O7粉体；
（3）将合成好的BaTi0.90Sn0.10O3粉体、Ca2LaMn2O7粉体，按照(1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7化学计量式配料；
（4）将步骤（3）配料好的原料，以无水乙醇为介质球磨15h，干燥，加入5%的PVA造粒，在150Mpa冷等静压成型；
（5）将步骤（4）成型的原料采用微波快速烧结，在1400℃保温30分钟，烧结成瓷；烧结后的样品加工成两面光滑的薄片，两面镀银电极制备成具有巨介电常数及电调特性的无铅铁电陶瓷材料。
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