CN106966720B - Bnt-bzn二元无铅电致应变陶瓷及制备 - Google Patents

Bnt-bzn二元无铅电致应变陶瓷及制备 Download PDF

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CN106966720B
CN106966720B CN201710254109.1A CN201710254109A CN106966720B CN 106966720 B CN106966720 B CN 106966720B CN 201710254109 A CN201710254109 A CN 201710254109A CN 106966720 B CN106966720 B CN 106966720B
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朱满康
位秋梅
李玲
任笑薇
郑木鹏
侯育冬
刘晶冰
王如志
汪浩
严辉
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Beijing University of Technology
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Abstract

BNT‑BZN二元无铅电致应变陶瓷、制备，属于电致应变陶瓷技术领域。该实验用两步法准备样品，首先以ZnO、Nb2O5为原料制备ZnNb2O6,之后再以Na2CO3、BaCO3、TiO2、Bi2O3及ZnNb2O6为原料，实现了无铅陶瓷(1‑x)Na0.5Bi0.5TiO3‑xBa(Zn1/ 3Nb2/3)O3的制备。在x＝5％时，该二元无铅铁电陶瓷表现大的电致应变，可以满足微位移器件对材料的要求。此时，电致应变S达到0.3％左右，是一种大应变的铁电陶瓷。

Description

BNT-BZN二元无铅电致应变陶瓷及制备
技术领域
本发明涉及一种具有大应变的新型(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3(即BNT-BZN)二元无铅铁电陶瓷，属于电致应变陶瓷技术领域。
技术背景
具有大的电场诱导应变的铁电陶瓷，具有体积小、承载力大、位移分辨率高、响应速度快，并且不发热、不产生噪音、低能耗、无电磁干扰等优点被广泛应用于微位移器，制动器，机敏结构及其它器件方面。铅基铁电陶瓷如Pb(Zr,Ti)O3,Pb(Mg,Nb)O3具有大的电致应变特性，一直占据电致应变器件市场的主导地位。但是其大的铅含量污染环境，有害人体健康，与环境友好型社会背道而驰。因此目前研究和开发无铅基铁电陶瓷具有很重要的意义。
随着技术的发展，微位移器件在精密光学、微电子学、航空航天、精密机床、微型马达、生物医学和扫描隧道效应显微镜等高技术领域的需求量日益增长，对精密元器件在加工过程中的定位精确性提出了更高要求。然而，外界环境因素如：温度、震动、噪声的变化都会对器件的微加工造成影响。因此，电致伸缩材料在微驱动和微控制技术中占有愈来愈重要的地位，引起国内外科研人员的广泛关注，获得了高度重视。目前，研究得最多的电致伸缩陶瓷是弛豫型铁电体陶瓷材料。虽然电致伸缩效应在固体电介质中普遍存在，但是其大小不同。从应用上看，要求电致伸缩材料在相对较低的电场条件下就能产生相对较大的应变，而且应变与电场的关系没有滞后，重复性好，同时还要求温度效应小。由于应变正比于介电常数的平方，又由于铁电体在其相变温度附近具有很大的介电常数，所以铁电体在其相变温度附近应该有较大的应变。
电致伸缩是一个四阶张量，存在于各种对称性的固体中；它是离子偏离平衡位置生产极化的一个标志，从而形成晶格常数的变化，即产生应变。自从Cross等在0.9Pb(Mg1/ 3Nb2/3)O3–0.1PbTiO3弛豫铁电体中观察到大的电致伸缩以来，铁电体成为制作致动器和微位移器的关键材料之一。近年来，研究者一直在无铅铁电体系中寻找具有大应变、小滞后和高温度稳定性的电致伸缩材料。
Bi1/2Na1/2TiO3(NBT)是一种ABO3型复合钙钛矿结构的铁电材料，具有良好的温度稳定性，优异的铁电性能，一种典型的A位复合钙钛矿结构弛豫铁电体。早在1998年，Chiang等在NBT–BT体系中观察到0.25％的小滞后电致应变。Jo等提出，NBT基体系大的电致应变，是由于NBT基体系中存在特殊的极性微区(polar nanoregions，PNRs)，施加电场后转变为铁电态，而电场撤除后恢复到极化前的状态。Han等将NBT基体系的PNRs分为非遍历态(低温)和遍历态(高温)：遍历态PNRs只能在电场的诱导下形成长程序，但电场撤除后则恢复非极性平衡态，从而产生无滞后的大电致应变。目前，遍历态与非遍历态之间的转变已成为解释NBT基体系介电和铁电行为的主要观点。为获得大的、无滞后的电致应变，研究者致力于获得具有非遍历态与遍历态PNRs共存结构的NBT基体系。
基于上面的考虑，我们以Na0.5Bi0.5TiO3为基体材料，加入立方相的Ba(Zn1/3Nb2/3)O3构成二元无铅固溶体系(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3。之前的大量研究表明在室温下样品处于遍历与非遍历态共存时能够达到大的应变。Ba(Zn1/3Nb2/3)O3是一种B位无序复合钙钛矿，它的加入主要是为了调节TF-R(遍历相与非遍历相的转变温度)，即通过改变Ba(Zn1/3Nb2/3)O3的百分含量进而调节TF-R使其逐渐往室温靠近，同时，Ba(Zn1/3Nb2/3)O3的无序结构，能影响Na0.5Bi0.5TiO3的离子分布结构，对PNRs的状态进行调制。通过这种设计，我们希望构造处于遍历与非遍历的共存态的铁电陶瓷，获得具有大的电致应变材料。
发明内容
本发明的目的是获得一种大电致应变的新型BNT基多元无铅铁电陶瓷体系。为达到发明目的，本发明通过引进钙钛矿结构Ba(Zn1/3Nb2/3)O3，与Bi0.5Na0.5TiO3形成二元无铅体系，以便在室温附近获得遍历态与非遍历态共存的弛豫铁电体。
本发明得到的无铅铁电陶瓷，化学通式为(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3，0<x≤0.06，优选0.05。体系具有三方和赝立方钙钛矿相共存结构。
本发明采用传统的陶瓷制备工艺，采用两步法制备样品：
(1)以ZnO、Nb2O5为原料制备ZnNb2O6，制备时煅烧温度为1000℃，保温4h；
(2)制备通式为(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3的无铅铁电陶瓷，采用的原料为化学纯或电子级Na2CO3、Bi2O3、TiO2、BaCO3及步骤(1)制备的ZnNb2O6，具体制备方法为，根据化学通式的化学摩尔计量比称量原料，将原料在乙醇中球磨12h，以使原料充分混合均匀，将混合均匀的原料烘干后装入氧化铝坩埚内，在800-950℃进行煅烧，保温时间4h；煅烧合成的粉料再经过12h的球磨磨细，烘干，掺入黏结剂PVB，压制成型(如在300MPa的压力下压制成直径为11.5mm的圆片)；所得坯体在650℃排胶后，以3℃/min的速率升温至1100℃～1200℃进行烧结，保温1～4h，获得Na0.5Bi0.5TiO3-Ba(Zn1/3Nb2/3)O3陶瓷。
烧结后的陶瓷片被上银电极，用于对样品进行各项性能的测试。
本发明通过构建(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3二元无铅固溶体，获得了电致应变S为0.29％的应变材料，实现了与铅基0.9Pb(Mgl/3Nb2/3)O3-0.1PbTiO3陶瓷应变性能可比拟的无铅铁电陶瓷。
附图说明
采用配有电致伸缩的铁电测试仪(Premier II,Radiant Technologies,USA)配合MTI 2100型光纤位移测试仪，测试电致应变。
图1为本发明成分组成为x＝5％电滞伸缩曲线。
具体实施方式
下面结合实施例对本发明做进一步说明，但本发明并不限于以下实施例。
本发明采用传统的陶瓷制备工艺，采用两步法制备样品，首先以ZnO、Nb2O5为原料制备ZnNb2O6,将原料在乙醇中球磨12h，充分混合原料，然后将混合均匀的原料烘干后放入氧化铝坩埚内，在1000℃的条件下进行煅烧，保温时间4h。制备本发明所述的通式为(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3的无铅铁电陶瓷，可以采用化学纯或电子级Na2CO3，Bi2O3，TiO2，BaCO3，及第一步制备的ZnNb2O6等为原料，按照传统的陶瓷制备工艺制得。具体制备方法为，根据化学通式和化学计量比称量原料，将原料在乙醇中球磨12h，以使原料充分混合均匀，将混合均匀的原料烘干后装入氧化铝坩埚内，在800-950℃进行煅烧，保温时间4h。煅烧合成的粉料再经过12h的球磨磨细。
在烘干的粉料中加粘结剂，在300Mpa的压力下成型，压制成直径11.5mm，厚度1.5mm左右的成型物。将成型物排胶，最后在1100-1200℃下烧结4h，烧结后的陶瓷片被上银电极然后对样品进行各项性能的测试。
按照上述方法制备的无铅铁电陶瓷的配方如下：
实施例1(对比例)：
配方：
Na0.5Bi0.5TiO3
工艺：煅烧温度850℃，烧结温度1150℃。
实施例2：
配方：
0.98Na0.5Bi0.5TiO3-0.02Ba(Zn1/3Nb2/3)O3
工艺：煅烧温度850℃，烧结温度1150℃。
实施例3：
配方：
0.96Na0.5Bi0.5TiO3-0.04Ba(Zn1/3Nb2/3)O3
工艺：煅烧温度850℃，烧结温度1150℃。
实施例4：
配方：
0.95Na0.5Bi0.5TiO3-0.05Ba(Zn1/3Nb2/3)O3
工艺：煅烧温度850℃，烧结温度1150℃。
实施例5：
配方：
0.94Na0.5Bi0.5TiO3-0.06Ba(Zn1/3Nb2/3)O3
工艺：煅烧温度850℃，烧结温度1150℃。
各实施例性能表：
Figure BDA0001272886560000061

Claims (1)

1.一种二元无铅陶瓷材料的应用，作为电致应变材料，陶瓷材料的组成通式可用(1-x)Na0.5Bi0.5TiO3-xBa(Zn1/3Nb2/3)O3表示，体系具有三方和赝立方钙钛矿相共存结构，Ba(Zn1/ 3Nb2/3)O3的摩尔分数x为0.05，在室温附近获得遍历态与非遍历态共存的弛豫铁电体。
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