CN107721411A - 一种大电致应变的无铅bnt‑bt基体系 - Google Patents
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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
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。
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、检测装置和控制系统。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:
Claims (4)
1.一种大电致应变的无铅BNT-BT基体系,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,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,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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