CN107721411B - 一种大电致应变的无铅bnt-bt基体系陶瓷 - Google Patents

一种大电致应变的无铅bnt-bt基体系陶瓷 Download PDF

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CN107721411B
CN107721411B CN201711071198.2A CN201711071198A CN107721411B CN 107721411 B CN107721411 B CN 107721411B CN 201711071198 A CN201711071198 A CN 201711071198A CN 107721411 B CN107721411 B CN 107721411B
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朱满康
位秋梅
李玲
郑木鹏
侯育冬
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Abstract

一种大电致应变的无铅BNT‑BT基体系，属于无铅铁电陶瓷材料领域。化学通式(1‑x)(Bi1/ 2Na1/2)TiO3‑xBaTiO3‑yBa(Zn1/3Nb2/3)O3，x＝0.06‑0.09，0<y≤0.02，采用两步法准备样品，首先以ZnO或(MgCO3)4.Mg(OH)2.5H2O与Nb2O5结合制备ZnNb2O6(MgNb2O6)。之后再以Na2CO3、BaCO3、TiO2、Bi2O3及ZnNb2O6(MgNb2O6)为原料，制备三元无铅铁电陶瓷。获得了大电致应变，可以满足微位移器件对材料的要求。

Description

一种大电致应变的无铅BNT-BT基体系陶瓷
技术领域
本发明涉及一种无铅铁电陶瓷材料领域，尤其涉及一种大电致应变的无铅BNT-BT基体系陶瓷。
技术背景
微位移技术是超精密加工及检测中的一项关键技术，包括微位移器件、检测装置和控制***。随着时代的发展，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，微位移器件在高技术领域的需求量日益增长，在微驱动和微控制技术中占有愈来愈重要的地位。通过电场诱导能产生大应变的铁电陶瓷(电致伸缩陶瓷)，具有体积小、承载力大、位移分辨率高、响应速度快等优点被广泛应用于微位移器、传感器、制动器、机敏结构及其它器件方面，引起国内外科研人员的广泛关注。
电致伸缩是由电场中电介质的极化引起的，它是离子偏离平衡位置产生极化的一个标志，也是晶格常数的变化和产生应变的起源。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，铅基铁电体成为制作致动器和微位移器的关键材料。目前，铅基铁电陶瓷，如Pb(Zr1-xTix)O3、Pb(Mg1/3Nb2/3)O3等陶瓷都具有大的电致应变，并占据着电致应变器件市场。但是铅基陶瓷含有的大量铅，污染环境，有害人体健康，与环境友好型社会背道而驰。因此，无铅基铁电陶瓷成为目前开发新型电致应变材料的主要方向。
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。在这些电致伸缩材料中，组成为(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3(x＝0.06-0.09)的陶瓷处于准同型相界(MPB)，由于存在的纳米畴作为中间连接相，有助于极化的重新取向，表现出相对较大的应变而成为很多研究者青睐的研究对象。如Yi-ping Guo等在BNT中引入7％BaTiO3获得了大的电致应变(0.41％@60kV/cm)。另外，研究表明钙钛矿铁电体的极化主要来自氧和B位阳离子的极化，因此为了得到大应变，很多研究者广泛引入A或B位离子来改变MPB附近的(Bi1/2Na1/2)TiO3-BaTiO3陶瓷的有序度，其中B位行为对改善应变更有效，这是因为复合离子的无序分布更能使(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3(x＝0.06-0.09)趋向于弛豫化，并增强铁电相与弛豫相之间的转变行为，获得大的电致应变。例如Shan-TaoZhang等用2％的K0.5Na0.5NbO3替代0.94Bi0.5Na0.5TiO3-0.06BaTiO3中Bi0.5Na0.5TiO3，获得了0.45％的小滞后电致应变。Fei-fei Wang等人发现，对(0.935-x)Bi0.5Na0.5TiO3–0.065BaTiO3–xSrTiO3陶瓷，当x＝0.22获得了大的电致应变(0.2％@40kV/cm)。Pin-Yi Chen等人发现，在(1-x)(Bi0.5Na0.5)TiO3–xBaTiO3陶瓷中，当x＝0.07时获得了大的电致应变(0.18％@40kV/cm)。
上述研究多是将铁电体引入(Bi1/2Na1/2)TiO3-BaTiO3，以调节其电致应变行为。本发明提出，将B位复合钙钛矿结构顺电体Ba(B1/3Nb2/3)O3(B＝Zn或Mg)引入到(1-x)(Bi1/ 2Na1/2)TiO3-xBaTiO3(x＝0.06-0.09)，以调制准同型相界附近的组成的离子分布，进而改善弛豫行为，获得大的电致应变。本发明所提及的Ba(B1/3Nb2/3)O3(B＝Zn或Mg)包括Ba(Zn1/ 3Nb2/3)O3(BZN)和Ba(Mg1/3Nb2/3)O3(BMN)，是二种B位离子复合钙钛矿顺电体，在室温下具有立方结构，其B位无序结构可以调节(Bi1/2Na1/2)TiO3-BaTiO3的弛豫行为，拓宽弛豫行为存在的温度范围，从而获得温度稳定的电致应变。本发明构建了(Bi1/2Na1/2)TiO3-BaTiO3-Ba(B1/ 3Nb2/3)O3(B＝Zn或Mg)三元无铅铁电陶瓷，构造出铁电相与弛豫相共存的结构，获得具有大的电致应变。
发明内容
本发明的目的是获得一种具有大电致应变的新型(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3(x＝0.06-0.09)基多元无铅铁电陶瓷。为此，本发明采用的方法是通过引入B位复合钙钛矿结构顺电体Ba(B1/3Nb2/3)O3(B＝Zn或Mg)，与(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3(x＝0.06-0.09)形成三元无铅铁电陶瓷，以获得铁电相与弛豫相共存的弛豫铁电体。
本发明采用传统的陶瓷制备工艺，通过两步法制备(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3(B＝Zn或Mg)陶瓷。
首先将ZnO或(MgCO3)4·Mg(OH)2·5H2O与Nb2O5结合制备ZnNb2O6或MgNb2O6：根据ZnNb2O6或MgNb2O6化学通式的摩尔计量比称量原料，将原料在乙醇中球磨，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800-900℃进行煅烧，保温时间2-6h；
其次，采用化学纯Na2CO3、Bi2O3、TiO2、BaCO3及第一步制备的ZnNb2O6或MgNb2O6为原料，按化学通式(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3(x＝0.06～0.09，0<y≤0.02，B＝Zn或Mg)的摩尔计量比称量原料，将原料在乙醇中球磨，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℃～900℃进行煅烧，保温时间3～6h；煅烧合成的粉料再经过球磨磨细，烘干,掺入黏结剂PVB，在300～400MPa的压力下压制成型；坯体排胶后，升温至1100℃～1200℃进行烧结，保温4～8h，获得(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3(x＝0.06～0.09，0<y≤0.02，B＝Zn或Mg)陶瓷。
烧结后的陶瓷片被上银电极，用于对(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/ 3Nb2/3)O3(x＝0.06-0.09，0<y≤0.02，B＝Zn或Mg)样品进行各项性能的测试。
本发明通过在(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3(x＝0.06-0.09)中引入Ba(B1/3Nb2/3)O3(B＝Zn或Mg)构成(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3(x＝0.06-0.09，0<y≤0.02，B＝Zn或Mg)三元无铅铁电陶瓷，进而获得大的电致应变；这种优异的场致应变性能，使其在无铅固体致动器中具有相当大的应用前景。尤其在0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3-0.01Ba(Zn1/3Nb2/3)O3陶瓷中获得了0.39％的大电致应变S(％)，在
0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3-0.01Ba(Mg1/3Nb2/3)O3陶瓷中获得了0.37％的大电致应变S(％)，实现了与铅基0.9Pb(Mgl/3Nb2/3)O3-0.1PbTiO3陶瓷可比拟的应变性能。
附图说明
采用X射线衍射仪测试陶瓷的相结构；采用配备美国MTI公司2100型光纤传感器的美国Radiant Technologies公司Premier II型铁电测试仪测试电致应变。
图1为本发明0.94(Bi1/2Na1/2)TiO3-0.06BaTiO3-0.0075Ba(Zn1/3Nb2/3)O3和0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3-0.01Ba(Zn1/3Nb2/3)O3陶瓷的XRD图，表明该陶瓷具有纯钙钛矿结构，并表现出三方-四方共存特征。
图2为本发明成分组成为0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3-0.01Ba(Mg1/3Nb2/3)O3在80kV/cm条件下的应变量为0.37％的电滞伸缩曲线。
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，首先第一步以ZnO或(MgCO3)4·Mg(OH)2·5H2O分别于Nb2O5结合制备ZnNb2O6(MgNb2O6),其制备方法为：根据化学通式的化学计量比称量原料，将原料在乙醇中球磨，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800-900℃进行煅烧，保温时间2-6h。本发明所述的最终通式为(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3(B＝Zn或Mg)的无铅铁电陶瓷，可以采用化学纯Na2CO3，Bi2O3，TiO2，BaCO3，及第一步制备的ZnNb2O6(MgNb2O6)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，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℃-900℃进行煅烧，保温时间4h。煅烧合成的粉料再经过球磨磨细。在烘干的粉料中加粘结剂，在300-400Mpa的压力下压制成型。将成型物进行排胶，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(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(Zn1/3Nb2/3)O3(x＝0.06-0.09，0<y≤0.02)和(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(Mg1/3Nb2/3)O3(x＝0.06-0.09，0<y≤0.02)的配比如下：
对比例：
成分：0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3
工艺：采用化学纯Na2CO3，Bi2O3，TiO2，BaCO3为原料，按通式(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3的化学计量比称量原料；将原料在乙醇中球磨，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℃进行煅烧，保温时间4h；煅烧合成的粉料再经过球磨磨细，在烘干的粉料中加粘结剂，在400Mpa的压力下压制成型；将成型物排胶，最后在1100℃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。
实施例1：
成分：0.94(Bi1/2Na1/2)TiO3-0.06BaTiO3-0.0075Ba(Zn1/3Nb2/3)O3
工艺：首先将ZnO与Nb2O5结合，制备ZnNb2O6；其制备方法为：根据化学通式ZnNb2O6的化学摩尔计量比称量原料，将原料在乙醇中球磨，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℃进行煅烧，保温时间4h。其次，采用化学纯Na2CO3，Bi2O3，TiO2，BaCO3及所制备的ZnNb2O6等为原料，按通式(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3(B＝Zn)的化学摩尔计量比称取原料；将原料在乙醇中球磨，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900℃进行煅烧，保温时间4h。煅烧合成的粉料再经过球磨磨细。在烘干的粉料中加粘结剂，在350Mpa的压力下压制成型。将成型物进行排胶，最后在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。
实施例2：
成分：0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3-0.01Ba(Zn1/3Nb2/3)O3
工艺：ZnNb2O6煅烧温度850℃，保温时间2h；通式陶瓷的煅烧温度850℃烧结温度1150℃，保温均为4h，压力300MPa，其他同实施例1。
实施例3：
成分：0.91(Bi1/2Na1/2)TiO3-0.09BaTiO3-0.02Ba(Zn1/3Nb2/3)O3
工艺：ZnNb2O6煅烧温度800℃，保温时间3h；通式陶瓷的煅烧温度800℃烧结温度1000℃，保温均为2h，压力300MPa，其他同实施例1。
实施例4：
成分：0.92(Bi1/2Na1/2)TiO3-0.08BaTiO3-0.0075Ba(Mg1/3Nb2/3)O3
工艺：MgNb2O6煅烧温度900℃，保温时间3h；通式陶瓷的煅烧温度800℃烧结温度1150℃，保温均为4h，压力400MPa，其他同实施例1(同时将ZnO替换为(MgCO3)4·Mg(OH)2·5H2O，将ZnNb2O6替换为MgNb2O6)。
实施例5：
成分：0.93(Bi1/2Na1/2)TiO3-0.07BaTiO3-0.01Ba(Mg1/3Nb2/3)O3
工艺：MgNb2O6煅烧温度850℃，保温时间4h；通式陶瓷的煅烧温度850℃烧结温度1150℃，保温均为4h，压力300MPa，其他同实施例1(同时将ZnO替换为(MgCO3)4·Mg(OH)2·5H2O，将ZnNb2O6替换为MgNb2O6)。
实施例6：
成分：0.94(Bi1/2Na1/2)TiO3-0.06BaTiO3-0.02Ba(Mg1/3Nb2/3)O3
工艺：MgNb2O6煅烧温度800℃，保温时间2h；通式陶瓷的煅烧温度900℃烧结温度1150℃，保温均为3h，压力350MPa，其他同实施例1(同时将ZnO替换为(MgCO3)4·Mg(OH)2·5H2O，将ZnNb2O6替换为MgNb2O6)。
对比例及实施例性能表：
Figure GDA0002697374330000071

Claims (4)

1.一种大电致应变的无铅BNT-BT基体系陶瓷，其特征在于，通过引入B位复合钙钛矿结构顺电体Ba(B1/3Nb2/3)O3，与(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3形成三元无铅铁电陶瓷，其化学通式(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3，B＝Zn或Mg，x＝0.06-0.09，0<y≤0.02。
2.按照权利要求1所述的一种大电致应变的无铅BNT-BT基体系陶瓷，其特征在于，大电致应变的无铅BNT-BT基体系具有纯钙钛矿结构，且三方-四方共存。
3.按照权利要求1所述的一种大电致应变的无铅BNT-BT基体系陶瓷，其特征在于，大电致应变的无铅BNT-BT基体系为铁电相与弛豫相共存的弛豫铁电体。
4.制备权利要求1所述的大电致应变的无铅BNT-BT基体系陶瓷的方法，其特征在于，采用传统的陶瓷制备工艺，通过两步法制备；
首先将ZnO或(MgCO3)4·Mg(OH)2·5H2O与Nb2O5结合制备ZnNb2O6或MgNb2O6：根据ZnNb2O6或MgNb2O6化学通式的摩尔计量比称量原料，将原料在乙醇中球磨，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800-900℃进行煅烧，保温时间2-6h；
其次，采用化学纯Na2CO3、Bi2O3、TiO2、BaCO3及第一步制备的ZnNb2O6或MgNb2O6为原料，按化学通式(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3的摩尔计量比称量原料，将原料在乙醇中球磨，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℃～900℃进行煅烧，保温时间3～6h；煅烧合成的粉料再经过球磨磨细，烘干,掺入黏结剂PVB，在300～400MPa的压力下压制成型；坯体排胶后，升温至1100℃～1200℃进行烧结，保温4～8h，获得(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3-yBa(B1/3Nb2/3)O3陶瓷。
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