CN105884350B - 一种锆钛酸钡钙无铅压电陶瓷材料及其制备方法 - Google Patents

一种锆钛酸钡钙无铅压电陶瓷材料及其制备方法 Download PDF

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CN105884350B
CN105884350B CN201610218671.4A CN201610218671A CN105884350B CN 105884350 B CN105884350 B CN 105884350B CN 201610218671 A CN201610218671 A CN 201610218671A CN 105884350 B CN105884350 B CN 105884350B
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zirconate titanate
free piezoceramic
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黄新友
殷佳
高春华
岳振星
李军
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Abstract

本发明涉及无机非金属材料技术领域，特指一种锆钛酸钡钙无铅压电陶瓷材料。配方组成包括：(Ba0.85Ca0.15)(Ti0.9Zr0.1)O391～98wt.％，BiFeO30.1～7.0wt.％，Bi2WO60.01～1wt.％,Ba(Yb1/2Nb1/2)O30.1～4wt.％,Co2O30.01～1.8wt.％；其中(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、它采用压电陶瓷普通化学原料，制备得到无铅、无镉的高压电性能的无铅压电陶瓷，还能大大降低压电陶瓷的烧结温度，适合于制备压电陶瓷传感器，能大大降低压电陶瓷的成本。

Description

一种锆钛酸钡钙无铅压电陶瓷材料及其制备方法
技术领域
本发明涉及无机非金属材料技术领域，特指一种锆钛酸钡钙无铅压电陶瓷材料。它采用压电陶瓷普通化学原料，制备得到无铅、无镉的高压电性能的无铅压电陶瓷，还能大大降低压电陶瓷的烧结温度，该压电陶瓷适合于制备压电陶瓷传感器，能大大降低压电陶瓷的成本，符合压电陶瓷的发展方向，在一些领域应用中能取代含铅压电陶瓷，并且在制备和使用过程中不污染环境。
背景技术
压电材料是一种能进行能量转换的新型功能材料，它能够实现机械能与电能之间的转换，随着电子科技与信息技术的快速发展，压电材料在人们生活的各个领域被普及开来，并且在涉及到军事以及国家安全也有很重要的应用。随着通讯、电子和医疗卫生等行业的飞速发展，对电子元器件小型化、功能化、低成本和高稳定性等要求越来越高。在过去压电材料的发展历程中，锆钛酸铅(Pb(Zr，Ti)O3)基二元系或多元系压电材料体系占据着主导地位，但这些压电材料中含有大量的铅(Pb)元素，而铅是一种在高温下易挥发的金属元素，对人类的身体健康和生存环境存在巨大的危害，基于此，无铅压电陶瓷的研究是一个必然趋势。在无铅压电陶瓷中，钛酸钡(BaTiO3)是最早发现的无铅压电陶瓷材料，也是目前研究相对成熟的无铅压电陶瓷材料，具有广阔的应用前景。但在实际应用过程中，BaTiO3陶瓷也存在一些问题，比如居里温度低(约120℃)，压电性能不高(约190pC/N)，工作温区窄，无法应用于大功率的换能器等方面；同时该压电陶瓷的稳定性欠佳，烧结困难，烧结温度一般要高达1300℃～1350℃。近年来，掺杂改性BaTiO3陶瓷的研究一直是国内外压电陶瓷领域的研究重点之一，通过在BaTiO3陶瓷中加入第二组元或多元组分可以得到较高压电性能的无铅的压电陶瓷材料。有研究者采用了CaTiO3-BaZrO3-BaTiO3复合形成固溶体，使其压电性能得到很大的提高，采用该方法得到的CaTiO3-BaZrO3-BaTiO3基无铅压电陶瓷的压电系数(d33)为482PC/N，径向机电耦合系数(KP)为0.48，但是，其居里温度为90℃左右，其压电陶瓷的烧结温度偏高(1500～1600℃)，该体系无铅压电陶瓷很难得到应用。因此,寻找出一种高压电性能、较高居里温度又能显著地降低烧结温度的有效方法，是一个重要的研究课题。
发明内容
本发明的目的是提供一种高性能锆钛酸钡钙无铅压电陶瓷材料。
本发明的目的是这样来实现的：
所述高性能锆钛酸钡钙无铅压电陶瓷配方组成包括：(Ba0.85Ca0.15)(Ti0.9Zr0.1)O391～98wt.％，BiFeO3 0.1～7.0wt.％，Bi2WO6 0.01～1wt.％,Ba(Yb1/2Nb1/2)O30.1～4wt.％,Co2O3 0.01～1.8wt.％；其中(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/ 2Nb1/2)O3分别采用常规的化学原料以固相法合成。
本发明的介质中所用的(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3是采用如下工艺制备的：将常规的化学原料BaCO3、CaCO3、TiO2、ZrO2按0.85：0.15：0.9：0.1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1350-1390℃保温120分钟，固相反应合成(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3，冷却后研磨过200目筛，备用。
本发明的介质中所用的Bi2WO6是采用如下工艺制备的：将常规的化学原料Bi2O3和WO3按1：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于850℃保温120分钟，冷却后得到Bi2WO6,研磨过200目筛，备用。
本发明的介质中所用的BiFeO3是采用如下工艺制备的：将常规的化学原料Bi2O3、Fe2O3按1/2：1/2摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于800-900℃保温120分钟，固相反应合成BiFeO3，冷却后研磨过200目筛，备用。
本发明的介质中所用的Ba(Yb1/2Nb1/2)O3的制备过程包括：将常规的化学原料BaCO3、Yb2O3、Nb2O5按1：1/4：1/4摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1250-1280℃保温120-180分钟，固相反应合成Ba(Yb1/2Nb1/2)O3，冷却后研磨过200目筛，备用。
本发明采用如下的陶瓷介质制备工艺：首先采用常规的化学原料用固相法分别合成(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3，然后按配方配料将配合料球磨粉碎混合，进行烘干后，加入粘合剂造粒，再压制成生坯片，然后在空气中进行排胶和烧结，获得高性能的压电陶瓷，被银电极，极化，然后测性能。
上述无铅压电陶瓷的配方最好采用下列二种方案：
(Ba0.85Ca0.15)(Ti0.9Zr0.1)O392～96wt.％，BiFeO30.1～5.0wt.％，Bi2WO60.01～0.8wt.％,Ba(Yb1/2Nb1/2)O30.1～3.8wt.％，Co2O3 0.03～1.6wt.％。
(Ba0.85Ca0.15)(Ti0.9Zr0.1)O392～95wt.％，BiFeO30.1～5.5wt.％，Bi2WO30.01～0.8wt.％,Ba(Yb1/2Nb1/2)O30.1～3.5wt.％，Co2O3 0.03～1.5wt.％。
本发明与现有技术相比，具有如下优点：
1、本专利的介质采用如下制备工艺：首先分别合成(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO3、Ba(Yb1/2Nb1/2)O3，然后按照配方配料，球磨混合，干燥，加入一定量的PVA溶液，造粒，干压成型，烧结，被银电极，极化，测试性能。
2、所制备的压电陶瓷的压电应变常数(d33)较高，可以达到320pC/N以上；径向机电耦合系数(Kp)较高，可以达到35％以上；介电常数(ε)较高,可以达到2500以上；居里温度(Tc)较高，可以达到135℃以上；介质损耗(tanδ)小于0.02；烧结温度较低，烧结温度不大于1360℃；使用过程中性能稳定性好，安全性高，对环境无污染。
3、主要原料采用压电陶瓷原料即可制造出本发明的高性能的无铅压电陶瓷。
具体实施方式
现在结合实施例对本发明作进一步的描述。表1给出本发明的实施例共4个试样的配方。
本发明的实施例共4个试样的配方的主要原料采用压电陶瓷原料，在制备时首先采用常规的化学原料用固相法分别合成(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO3、Ba(Yb1/2Nb1/2)O3，然后按上述配方配料，将配好的料用无水乙醇采用行星球磨机球磨混合，料：球：无水乙醇＝1：3：(0.6～1.0)(质量比)，球磨4～8小时后，烘干得干粉料，在干粉料中加入占其重量8～10％的浓度为10％(重量百分比)的聚乙烯醇溶液，进行造粒，混研后过40目筛，再在20～30Mpa压力下进行干压成生坯片，然后在温度为1330～1360℃下保温2～3小时进行排胶和烧结，再在780～800℃下保温15分钟进行烧银，形成银电极，并在硅油中100℃极化，极化电场为3000～4000伏/mm，极化时间为15～20分钟；极化完毕，经过老化48小时，测试其性能。
上述各配方试样的性能列于表2。从表2可以看出所制备的压电陶瓷的压电应变常数(d33)较高，可以达到320pC/N以上；径向机电耦合系数(Kp)较高，可以达到35％以上；介电常数(ε)较高,可以达到2500以上；居里温度(Tc)较高，可以达到135℃以上；介质损耗(tanδ)小于0.02；烧结温度较低，烧结温度为1360℃以下。
表1 本发明的实施例共4个试样的配方
注:BCTZ是(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3的简称
表2 各配方试样的性能
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于所述锆钛酸钡钙无铅压电陶瓷材料配方组成为：(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3 91～98wt.％，BiFeO3 0.1～7.0wt.％，Bi2WO60.01～1wt.％,Ba(Yb1/2Nb1/2)O3 0.1～4wt.％,Co2O3 0.01～1.8wt.％。
2.如权利要求1所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于：所述(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3分别采用常规的化学原料以固相法合成。
3.如权利要求1或2所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于，所述(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3是采用如下工艺制备的：将常规的化学原料BaCO3、CaCO3、TiO2、ZrO2按0.85：0.15：0.9：0.1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1350-1390℃保温120分钟，固相反应合成(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3，冷却后研磨过200目筛，备用。
4.如权利要求1或2所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于所述的Bi2WO6是采用如下工艺制备的：将常规的化学原料Bi2O3和WO3按1：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于850℃保温120分钟，冷却后得到Bi2WO6，研磨过200目筛，备用。
5.如权利要求1或2所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于所述的BiFeO3是采用如下工艺制备的：将常规的化学原料Bi2O3、Fe2O3按1/2：1/2摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于800-900℃保温120分钟，固相反应合成BiFeO3，冷却后研磨过200目筛，备用。
6.如权利要求1或2所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于所述的Ba(Yb1/2Nb1/2)O3的制备过程包括：将常规的化学原料BaCO3、Yb2O3、Nb2O5按1：1/4：1/4摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1250-1280℃保温120-180分钟，固相反应合成Ba(Yb1/2Nb1/2)O3，冷却后研磨过200目筛，备用。
7.如权利要求1所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于所述锆钛酸钡钙无铅压电陶瓷材料配方组成为：(Ba0.85Ca0.15)(Ti0.9Zr0.1)O392～96wt.％，BiFeO30.1～5.0wt.％，Bi2WO60.01～0.8wt.％，Ba(Yb1/2Nb1/2)O30.1～3.8wt.％，Co2O30.03～1.6wt.％。
8.如权利要求1所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于所述锆钛酸钡钙无铅压电陶瓷材料配方组成为：(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3 92～95wt.％，BiFeO30.1～5.5wt.％，Bi2WO6 0.01～0.8wt.％，Ba(Yb1/2Nb1/2)O30.1～3.5wt.％，Co2O3 0.03～1.5wt.％。
9.如权利要求1所述的一种锆钛酸钡钙无铅压电陶瓷材料，其特征在于：所述锆钛酸钡钙无铅压电陶瓷材料压电常数(d33 )较高，可以达到320pC/N以上；径向机电耦合系数较高，可以达到35％以上；介电常数(ε)较高,可以达到2500以上；居里温度(Tc)较高，可以达到135℃以上；介质损耗(tanδ)小于0.02；烧结温度较低，不大于1360℃。
10.如权利要求1所述的一种锆钛酸钡钙无铅压电陶瓷材料的制备方法，其特征在于：首先采用常规的化学原料用固相法分别合成(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3，然后按配方配料，将配好的料用无水乙醇采用行星球磨机球磨混合，按质量比料：球：无水乙醇＝1：3：(0.6～1.0)，球磨4～8小时后，烘干得干粉料，在干粉料中加入占干粉料重量8～10％的质量百分浓度为10％的聚乙烯醇溶液，进行造粒，混研后过40目筛，再在20～30MPa 压力下进行干压成生坯片，然后在温度为1330～1360℃下保温2～3小时进行排胶和烧结，再在780～800℃下保温15分钟进行烧银，形成银电极，并在硅油中100℃极化，极化电场为3000～4000伏/mm，极化时间为15～20分钟；极化完毕，经过老化48小时，测试其性能。
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