CN105732024A - 新型二元系K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3无铅压电陶瓷材料及制备 - Google Patents

新型二元系K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3无铅压电陶瓷材料及制备 Download PDF

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CN105732024A
CN105732024A CN201610035194.8A CN201610035194A CN105732024A CN 105732024 A CN105732024 A CN 105732024A CN 201610035194 A CN201610035194 A CN 201610035194A CN 105732024 A CN105732024 A CN 105732024A
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朱满康
胡彬彬
郭金键
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

新型二元系K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3无铅压电陶瓷材料及制备，属于钙钛矿结构压电陶瓷领域。材料用通式(1?x)K0.5Bi0.5TiO3?x BiMg0.5Zr0.5O3(0<x≤0.08)表示。该体系的煅烧温度为800℃?900℃，成型压力为150MPa～300Mpa，烧结温度为1040℃?1080℃。成功实现了对KBT无铅压电陶瓷压电性能的改良，在准同型相界附近，x＝0.01即组分为0.99K0.5Bi0.5TiO3?0.01BiMg0.5Zr0.5O3时有最大的d33＝65pC/N。

Description

新型二元系K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3无铅压电陶瓷材料及 制备
技术领域
本发明属于钙钛矿结构压电陶瓷领域，涉及一类新型的具有较高压电性能的二元K0.5Bi0.5TiO3基无铅压电陶瓷材料，具体是(1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0<x≤0.08)系无铅压电陶瓷材料组成及其制备方法。
技术背景
压电陶瓷指具有压电效应,能够将机械能和电能互相转换的一种功能陶瓷材料。作为一种电子陶瓷材料，它被广泛地用来制备传感器、压电换能器、压电驱动器等电子元器件，应用领域十分广泛，与我们的生活息息相关。特别是具有优异压电性能和高居里温度的锆钛酸铅Pb(Ti，Zr)O3陶瓷开发成功后，结构特征为ABO3型的铅基钙钛矿压电陶瓷发展甚为迅速，用它制作的压电滤波器、微位移器、驱动器和传感器等，被广泛应用于卫星广播、电子设备、生物以及航空航天等高新技术领域。
目前应用最广泛的锆钛酸铅(PbZrxTi1-xO3，简写为PZT)基陶瓷，是一种工艺成熟、性能优异稳定的钙钛矿结构压电陶瓷。然而，铅基压电陶瓷中PbO(或Pb3O4)的含量占原料总量的70％以上，如此高含量的铅在压电陶瓷制备、使用、废弃处理或回收过程中都会给生态环境和人类造成严重危害。随着社会各界对环境保护问题的重视，很多国家纷纷提出法令法规禁止含铅的压电铁电材料的使用，环境友好型无铅压铁电陶瓷已成为各国致力研发和关注的重要材料之一。
无铅压电陶瓷材料主要有钙钛矿、钨青铜和铋层状三种晶体结构类型。其中，钙钛矿结构Na0.5Bi0.5TiO3(简称为BNT)基体系是研究较多的无铅压电体系。但单纯NBT陶瓷的极化十分困难，存在较低的退极化温度，且难以消除，这就严重限制了它的实际应用。KBT即K0.5Bi0.5TiO3，室温下为四方相，与NBT十分相似，也是一种ABO3型钙钛矿结构的铁电材料，与NBT相比，KBT有更高的居里温度(TC＝380℃)和较低的矫顽场(Ec＝15kV/cm)，且不存在退极化温度，具有更广阔的应用前景。通过与其它钙钛矿结构化合物复合形成的多元固溶体系，可进一步改善KBT陶瓷的烧结和电学性能。
BiMg0.5Zr0.5O3(BMZ)是一种具有亚稳的类钙钛矿结构的化合物，难以合成。BMZ具有较低的容差因子，引入到四方结构的K0.5Bi0.5TiO3中可能与之形成准同型相界。因此，由KBT-BMZ构成的二元系压电陶瓷，可能具有良好的压电性能。
发明内容
本发明的目的是提供一种新型KBT基二元无铅压电陶瓷体系。
本发明一种KBT基二元无铅压电陶瓷体系，其特征在于，KBT基二元无铅压电陶瓷体系含有KBT、BMZ两种成分，其中，KBT为K0.5Bi0.5TiO3，BMZ为BiMg0.5Zr0.5O3；组成的通式表示为(1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0<x≤0.08)。
本发明采用BiMg0.5Zr0.5O3与K0.5Bi0.5TiO3构成二元固溶体系，形成具有四方钙钛矿相和赝立方钙钛矿相晶体结构共存的准同型相界。本发明得到的无铅压电陶瓷的化学通式为(1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0<x≤0.08，优选0.01)。
本发明采用传统的陶瓷制备工艺，所述通式为(1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3的无铅压电陶瓷采用的原料主要为化学纯或电子级K2CO3、Bi2O3、TiO2、ZrO2、4MgCO3·Mg(OH)2·5H2O等。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12小时，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3小时。煅烧合成的粉料再经过12小时的球磨磨细；将球磨磨细的粉末烘干然后加粘结剂，在150MPa-300MPa的压力下成型，然后将成型物排胶，最后在1040℃-1080℃下烧结4小时，得到无铅压电陶瓷体系。
烧结后的陶瓷片被上银电极，在120℃的硅油中，在4.5kV·mm-1的电压下极化30min。然后对样品进行各项性能的测试。
本发明通过KBT基二元固溶体系的构建，成功实现了对KBT无铅压电陶瓷压电性能的改良，该体系矫顽场在17kV/cm～31kV/cm之间随着二元体系组分的变化而改变，压电系数d33从17pC/N～65pC/N不等，在准同型相界附近，x＝0.01即组分为0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3时有最大的d33＝65pC/N。
附图说明
图1为本发明的化学组成为0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3，即x＝0.01时的电滞回线；
图2本发明的化学组成为0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3的44°～48°范围的X射线衍射谱，可以明显此处存在的四方结构与立方结构的衍射峰。
具体实施方式
以下将通过实施例对本发明进行详细描述，这些实施例只是出于示例性说明的目的，而非用于限定本发明。
制备本发明所述的通式为(1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3(0<x≤0.08)的无铅压电陶瓷，可以采用化学纯或电子级K2CO3，Bi2O3，TiO2，ZrO2，4MgCO3·Mg(OH)2·5H2O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12小时，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3小时。煅烧合成的粉料再经过12小时的球磨磨细。
球磨磨细的粉料烘干后加粘结剂，在150MPa-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1040℃-1080℃下烧结4小时，烧结后的陶瓷片被上银电极，在120℃的硅油中，在4.5kV·mm-1的电压下极化30min。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压电陶瓷的配方和性能如下：
对比例：
配方：
K0.5Bi0.5TiO3
工艺：
根据K0.5Bi0.5TiO3的配方称量原料，将原料在乙醇中球磨12小时，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3小时。煅烧合成的粉料再经过12小时的球磨磨细。在烘干的粉料中加粘结剂，在150MPa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1040℃下烧结4小时。
实施例1：
配方：
0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3
工艺：根据0.99K0.5Bi0.5TiO3-0.01BiMg0.5Zr0.5O3的配方称量原料，煅烧温度830℃，成型压力为190MPa，烧结温度1050℃；其他工艺条件与对比例相同。
实施例2：
配方：
0.97K0.5Bi0.5TiO3-0.03BiMg0.5Zr0.5O3
工艺：根据0.97K0.5Bi0.5TiO3-0.03BiMg0.5Zr0.5O3的配方称量原料，煅烧温度855℃，成型压力为230MPa，烧结温度1060℃；其他工艺条件与对比例相同。
实施例3：
配方：
0.95K0.5Bi0.5TiO3-0.05BiMg0.5Zr0.5O3
工艺：根据0.95K0.5Bi0.5TiO3-0.05BiMg0.5Zr0.5O3的配方称量原料煅烧温度870℃，成型压力为270MPa，烧结温度1070℃；其他工艺条件与对比例相同。
实施例4：
配方：
0.92K0.5Bi0.5TiO3-0.08BiMg0.5Zr0.5O3
工艺：根据0.92K0.5Bi0.5TiO3-0.08BiMg0.5Zr0.5O3的配方称量原料煅烧温度900℃，成型压力为300MPa，烧结温度1080℃；其他工艺条件与对比例相同。
表1各实施例性能表：

Claims (4)

1.一种KBT基二元无铅压电陶瓷体系，其特征在于，KBT基二元无铅压电陶瓷体系含有KBT、BMZ两种成分，其中，KBT为K0.5Bi0.5TiO3，BMZ为BiMg0.5Zr0.5O3；组成的通式为(1-x)K0.5Bi0.5TiO3-xBiMg0.5Zr0.5O3，0<x≤0.08。
2.按照权利要求1所述的一种KBT基二元无铅压电陶瓷体系，其特征在于，x＝0.01。
3.按照权利要求1或2所述的一种KBT基二元无铅压电陶瓷体系，其特征在于，BiMg0.5Zr0.5O3与K0.5Bi0.5TiO3形成二元固溶体系，形成具有四方钙钛矿相和赝立方钙钛矿相晶体结构共存的准同型相界。
4.一种制备权利要求1-3任一项所述的KBT基二元无铅压电陶瓷体系的方法，其特征在于，原料主要为化学纯或电子级K2CO3、Bi2O3、TiO2、ZrO2、4MgCO3·Mg(OH)2·5H2O，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12小时，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3小时。煅烧合成的粉料再经过12小时的球磨磨细；将球磨磨细的粉末烘干然后加粘结剂，在150MPa-300MPa的压力下成型，然后将成型物排胶，最后在1040℃-1080℃下烧结4小时，得到KBT基二元无铅压电陶瓷体系。
CN201610035194.8A 2016-01-19 2016-01-19 新型二元系K0.5Bi0.5TiO3–BiMg0.5Zr0.5O3无铅压电陶瓷材料及制备 Expired - Fee Related CN105732024B (zh)

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