CN105859283B - K0.5Bi0.5TiO3–BiNi0.5Zr0.5O3电致伸缩陶瓷材料及制备 - Google Patents

K0.5Bi0.5TiO3–BiNi0.5Zr0.5O3电致伸缩陶瓷材料及制备 Download PDF

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CN105859283B
CN105859283B CN201610299313.0A CN201610299313A CN105859283B CN 105859283 B CN105859283 B CN 105859283B CN 201610299313 A CN201610299313 A CN 201610299313A CN 105859283 B CN105859283 B CN 105859283B
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朱满康
郭金键
李玲
郑木鹏
侯育冬
刘晶冰
王如志
汪浩
严辉
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Abstract

K0.5Bi0.5TiO3–BiNi0.5Zr0.5O3电致伸缩陶瓷材料及制备，属于钙钛矿结构铁电陶瓷领域。用通式(1‑x)K0.5Bi0.5TiO3‑x BiNi0.5Zr0.5O3(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℃。该体系最大应变量在0.015‑0.077之间随着二元体系组分的变化而改变，动态压电系数d33 *从46‑113pC/N不等，并且x＝0.06时有最大的d33 *＝113pC/N和最大的应变Smax＝0.077％。

Description

K0.5Bi0.5TiO3–BiNi0.5Zr0.5O3电致伸缩陶瓷材料及制备
技术领域
本发明属于钙钛矿结构电致伸缩陶瓷领域，涉及一类新型的具有较大压电性能的二元K0.5Bi0.5TiO3基无铅压电陶瓷材料，具体是(1-x)K0.5Bi0.5TiO3-xBiNi0.5Zr0.5O3(0<x≤0.08)系无铅大电致伸缩陶瓷材料组成及其制备方法。
技术背景
1977年美国的L.E.Cross开始研究电致伸缩效应，并且得到了美国海军的大力支持。1979年L.E.Cross等人开发的新型电致伸缩材料妮镁酸铅((PMN)陶瓷获得了美国十大科技成果。电致伸缩陶瓷也是一种能够将电能和机械能互相转换的一种功能陶瓷材料。在发现电致伸缩材料以前，一般都是利用压电材料来制造电控位移器。但是与压电材料相比，电致伸缩有以下几个优势(1)老化性能好(2)不需要高温极化(3)不存在残余应变(4)基本无滞后，重复性比较好。这些优点使得电致伸缩效应在压力测量、连续可调激光器、双稳态光电器件等方面得到了很好的应用。随着近年来布里渊散射、次级光电效应研究、激光自聚焦等非线性光学的发展，人们研究出了电致伸缩谐振子和传感器，电致伸缩效应逐渐引起了越来越多的关注。
随着铁电/电致伸缩陶瓷的应用范围不断扩大，对材料的要求也必将日益苛刻。虽然铅基材料的性能非常卓越，但是含铅材料的主要成分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，环境友好型无铅压电/电致伸缩陶瓷已成为各国致力研发和关注的重要材料之一。
无铅铁电/电致伸缩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，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，KBT有更高的居里温度(TC＝380℃)和较低的矫顽场(Ec＝15kV/cm)，具有广阔的应用前景。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。
BiNi0.5Zr0.5O3(BNZ)是一种具有亚稳的类钙钛矿结构的化合物，难以合成。BNZ具有较低的容差因子，引入到四方结构的K0.5Bi0.5TiO3中可与之在x＝0.03处形成准同型相界，其压电铁电性能达到最优。并且，由KBT-BNZ构成的二元系电致伸缩陶瓷在准同型相界附近x＝0.06处，其电致伸缩性能达到最大。
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，其特征是陶瓷材料组成的通式可用(1-x)K0.5Bi0.5TiO3-xBiNi0.5Zr0.5O3(0<x≤0.08)表示。
为达到发明目的，本发明一种新型无铅电致伸缩陶瓷体系，其特征在于，含有KBT、BNZ两种成分，其中，KBT为K0.5Bi0.5TiO3，BNZ为BiNi0.5Zr0.5O3，BiNi0.5Zr0.5O3与K0.5Bi0.5TiO3形成二元固溶体系；以形成准同型相界；体系具有四方钙钛矿晶相和赝立方钙钛矿相共存的晶体结构。本发明得到的无铅压电陶瓷的化学通式为(1-x)K0.5Bi0.5TiO3-xBiNi0.5Zr0.5O3，0<x≤0.08，优选x＝0.06。
本发明采用传统的陶瓷制备工艺，所述通式为(1-x)K0.5Bi0.5TiO3-xBiNi0.5Zr0.5O3的无铅压电陶瓷可以采用的原料为化学纯或电子级K2CO3、Bi2O3、TiO2、ZrO2、NiO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至少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；在烘干的粉料中加粘结剂，在150MPa-300MPa的压力下成型，将成型物排胶，最后在1040℃-1080℃下烧结4 小时。
本发明通过KBT基二元固溶体系的构建，成功实现了对KBT无铅压电陶瓷电致伸缩性能的改良，该体系最大应变量在0.015-0.077之间随着二元体系组分的变化而改变，动态压电系数d33 *从46-113pC/N不等，并且在准同型相界(x＝0.03)附近x＝0.06即0.94K0.5Bi0.5TiO3-0.06BiNi0.5Zr0.5O3时有最大的d33 *＝113pC/N和最大的应变Smax＝0.077％。
附图说明
图1为本发明的化学组成为0.94K0.5Bi0.5TiO3-0.06BiNi0.5Zr0.5O3，即x＝0.06时的双极电致伸缩回线。
图2为本发明的化学组成为0.94K0.5Bi0.5TiO3-0.06BiNi0.5Zr0.5O3，即x＝0.06时的单极电致伸缩回线。
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-xBiNi0.5Zr0.5O3(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，NiO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。
在烘干的粉料中加粘结剂，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，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电致伸缩陶瓷的配方和性能如下：
对比例：
配方：
1.0K0.5Bi0.5TiO3-0BiNi0.5Zr0.5O3
工艺：根据配方称量原料，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：
0.99K0.5Bi0.5TiO3-0.01BiNi0.5Zr0.5O3
工艺：原料粉末煅烧温度830℃，成型压力为190MPa，成型后烧结温度1050℃；其他工艺条件与对比例相同。
实施例2：
配方：
0.98K0.5Bi0.5TiO3-0.03BiNi0.5Zr0.5O3
工艺：原料粉末煅烧温度855℃，成型压力为230MPa，成型后烧结温度1060℃；其他工艺条件与对比例相同。
实施例3：
配方：
0.94K0.5Bi0.5TiO3-0.06BiNi0.5Zr0.5O3
工艺：原料粉末煅烧温度870℃，成型压力为270MPa，成型后烧结温度1070℃；其他工艺条件与对比例相同。
实施例4：
配方：
0.92K0.5Bi0.5TiO3-0.08Bi Ni0.5Zr0.5O3
工艺：原料粉末煅烧温度900℃，成型压力为300MPa，成型后烧结温度1080℃；其他工艺条件与对比例相同。
各实施例性能表：

Claims (3)

1.一种无铅电致伸缩陶瓷材料，其特征在于，含有KBT、BNZ两种成分，其中，KBT为K0.5Bi0.5TiO3，BNZ为BiNi0.5Zr0.5O3，BiNi0.5Zr0.5O3与K0.5Bi0.5TiO3形成二元固溶体系；陶瓷材料的组成通式为(1-x)K0.5Bi0.5TiO3-xBiNi0.5Zr0.5O3，0<x≤0.08，材料具有四方钙钛矿晶相和赝立方钙钛矿相共存的晶体结构；
其制备方法：采用的原料为化学纯或电子级K2CO3、Bi2O3、TiO2、ZrO2、NiO，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至少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至少12小时的球磨磨细；在烘干的粉料中加粘结剂，在150MPa～300MPa的压力下成型，将成型物排胶，最后在1040℃～1080℃下烧结4小时。
2.按照权利要求1中所述的无铅电致伸缩陶瓷材料，其特征在于x＝0.06。
3.制备权利要求1中所述的无铅电致伸缩陶瓷材料的方法，其特征在于，采用的原料为化学纯或电子级K2CO3、Bi2O3、TiO2、ZrO2、NiO，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至少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至少12小时的球磨磨细；在烘干的粉料中加粘结剂，在150MPa～300MPa的压力下成型，将成型物排胶，最后在1040℃～1080℃下烧结4小时。
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