CN110128128B - 一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷及其制备方法 - Google Patents

一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷及其制备方法 Download PDF

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CN110128128B
CN110128128B CN201910582276.8A CN201910582276A CN110128128B CN 110128128 B CN110128128 B CN 110128128B CN 201910582276 A CN201910582276 A CN 201910582276A CN 110128128 B CN110128128 B CN 110128128B
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bismuth
piezoelectric ceramic
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CN110128128A (zh
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孙媛媛
杨华斌
刘笑
江民红
陈巧红
张秀云
黄蔚然
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Guilin University of Electronic Technology
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Abstract

本发明公开了一种具有零温度系数及高温稳定性的铁酸铋‑铝酸铋‑锌钛酸铋高温压电陶瓷及其制备方法，其组成通式为：xBi1.05FeO3‑yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3，其中P为Ba(W0.5Cu0.5)O3、CuO、Li2CO3中的一种或多种烧结助剂的组合；x、y、z、t、m表示摩尔分数，且0.50≤x≤0.80,0<y≤0.1,0<z≤0.20,0<t≤0.1,0<m≤0.1，其制备方法包括按组成通式配料、球磨、成型、排胶、烧结等工序，包括采用低温烧结助剂促进烧结、获得致密压电陶瓷的方法，制备出了具有超过680℃的居里温度和650℃的退极化温度、且获得了且压电常数d33＝20pC/N的压电陶瓷，该体系陶有望应用在航天航空等高温压电振动传感器领域。

Description

一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸 铋高温压电陶瓷及其制备方法
技术领域
本发明涉及可在航天航空等领域应用的高温压电陶瓷材料，具体是一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷及其制备方法。
背景技术
高温压电陶瓷作为振动传感器被广泛应用于航天航空、核能、石油勘探等领域，高温压电陶瓷的工作环境非常恶劣，因此对压电陶瓷的要求很高，如低介电损耗及高的温稳定性等，其中高温稳定性要求在高温工作环境下保持压电性能的稳定。BiFeO3具有高的居里温度(830℃)和大的剩余极化强度，理论计算表明BiFeO3具有良好的压电性能，但是纯BiFeO3存在烧结困难、漏电流高，烧结过程中钙钛矿结构不稳定，极易产生杂项等缺陷，导致该体系无法得到实际应用。Bi(Ti0.5Zn0.5)O3是一种具有高居里温度的四方相钙钛矿结构化合物，其与BiFeO3可形成固溶体，根据理论计算，两者的固溶体在单斜相0.4BZT-0.6BF成分处的TC可以达到1227℃左右，但Bi(Ti0.5Zn0.5)O3需在高温高压下合成。BiAlO3为三方相钙钛矿结构化合物，居里温度超过550℃，其从室温至550℃之间没有任何相变，具有非常高的温度稳定性。
发明内容
本发明的目的是针对现有技术的缺陷，提供一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷及其制备方法。本发明以BiFeO3-Bi(Ti0.5Zn0.5)O3为基体材料，通过添加适量的BiAlO3与其形成固溶体，对BiFeO3-Bi(Ti0.5Zn0.5)O3的温度系数进行调控，并采用添加烧结助剂降低烧结温度，获得致密、具有接近零温度系数的BiFeO3-Bi(Ti0.5Zn0.5)O3-BiAlO3压电陶瓷，其居里温度可达到Tc＝680℃，退极化温度达到Td＝650℃，且压电常数达到20pC/N，有望应用在高温压电振动传感器领域。
实现本发明目的的技术方案是：
一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷，其组成通式为：xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3，其中x、y、z、t、m表示摩尔分数，P为Ba(W0.5Cu0.5)O3、CuO、Li2CO3中的一种或多种烧结助剂的组合，且0.5≤x≤0.8,0<y≤0.10,0<z≤0.20,0<t≤0.1,0<m≤0.1。
所述具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷的制备方法，包括如下步骤：
(1)以分析纯Fe2O3、Bi2O3、TiO2、ZnO、Al2O3、Ba2CO3、W2O3、CuO、MnCO3、Li2CO3为原料，按照xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3进行配料，其中0.5≤x≤0.8,0<y≤0.10,0<z≤0.20,0<t≤0.1,0<m≤0.1，Bi元素过量5％为弥补烧结过程中Bi元素的挥发，P为Ba(W0.5Cu0.5)O3、CuO、Li2CO3中的一种或多种烧结助剂的组合，将混合粉末以无水乙醇为介质球磨24小时，100℃/12小时在烘箱中烘干、过筛，放入高铝坩埚中压实加盖，再放入密闭管式炉中通纯氧气以250℃/h的升温速率到850℃预烧，保温6小时合成，并降温冷却至200℃以下后取出备用；
(2)将步骤(1)合成的xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3，粉末以无水乙醇为介质进行二次球磨24小时，取出干燥，过200目筛；
(3)将过筛后的粉末加入质量百分比浓度为5％PVA的溶液造粒，在钢模中于100MPa下压制成型，模具内直径为1cm；
(4)成型的素片放入马弗炉中以30℃/h的升温速率缓慢升温至600℃，保温24小时排胶；然后以20℃/min的升温速率快速升温到970-1020℃，保温120分钟后随炉冷却至室温；
(5)将烧结后样品抛光成两面光滑、厚度1mm的薄片，披银电极，650℃/30分钟烧银后备用；
(6)将披银电极后的压电陶瓷片在硅油中极化，极化电场6000V/mm，极化温度150℃，时间30分钟，保持电场冷却至室温。
本发明的积极效果是：
本发明采用具有高居里温度的Bi(Ti0.5Zn0.5)O3与BiFeO3进行B位复合离子取代，以获得具有更高的居里温度和温度稳定性的压电陶瓷，并采用烧结助剂降低烧结温度促进烧结过程的进行，以获得更加致密的压电陶瓷。同时采用BiAlO3对温度系数进行调控，获得具有接近零温度系数的xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3压电陶瓷。采用此技术制备的xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3压电陶瓷，具有超过680℃的居里温度和650℃的退极化温度，且获得了且压电常数达到d33＝20pC/N的压电陶瓷，该技术具有重大突破和创新，并具有实用性。
具体实施方式
实施例1：
成分：0.80Bi1.05FeO3-0.05BiAlO3+0.15Bi(Ti0.5Zn0.5)O3+0.025Ba(W0.5Cu0.5)O3+0.01MnCO3，制备方法包括如下步骤：
(1)以分析纯Fe2O3、Bi2O3、TiO2、ZnO、Al2O3、BaCO3、W2O3、CuO、MnCO3为原料，按照0.80Bi1.05FeO3-0.05BiAlO3+0.15Bi(Ti0.5Zn0.5)O3+0.025Ba(W0.5Cu0.5)O3+0.01MnCO3进行配料，以无水乙醇为介质球磨24小时，在100℃/12小时烘干、过筛，放入高铝坩埚中加盖，再放入密闭通纯氧管式炉中以250℃/h的升温速率到850℃预烧，保温6小时合成，并降温冷却至200℃以下后取出。
(2)将步骤(1)合成的0.80Bi1.05FeO3-0.05BiAlO3+0.15Bi(Ti0.5Zn0.5)O3+0.025Ba(W0.5Cu0.5)O3+0.01MnCO3粉末以无水乙醇为介质进行二次球磨24小时，取出干燥，过200目筛；
(3)将过筛后的粉末加入质量百分比浓度为的5％PVA溶液造粒，在钢模中于100MPa下压制成型，模具内直径为1cm；
(4)成型的素片放入马弗炉中以60℃/h的升温速率缓慢升温至600℃，保温24小时排胶；然后以20℃/min的升温速率快速升温到990℃，保温120分钟后随炉冷却至室温；
(5)将烧结后样品抛光成两面光滑、厚度1mm的薄片，披银电极，650℃/30分钟烧银后备用；
(6)将披银电极后的压电陶瓷片在硅油中极化，极化电场6000V/mm，极化温度150℃，时间30分钟，保持电场冷却至室温。
性能测量结果如下：
d<sub>33</sub>(pC/N) Q<sub>m</sub> k<sub>p</sub>(％) ε<sub>r</sub> Tc(℃) T<sub>d</sub>(℃)
20 63.4 0.31 107 680 650
实施例2：
成分：0.75Bi1.05FeO3-0.05BiAlO3+0.20Bi(Ti0.5Zn0.5)O3+0.01Li2CO3+0.01MnCO3，以分析纯Fe2O3、Bi2O3、BaCO3、TiO2、ZnO、Al2O3、Li2CO3、MnCO3为原料，按照0.75Bi1.05FeO3-0.05BiAlO3+0.20Bi(Ti0.5Zn0.5)O3+0.01Li2CO3+0.01MnCO3进行配料，制备方法同实施例1，烧结温度为980℃。
性能测量结果如下：
Figure BDA0002113466260000031
Figure BDA0002113466260000041
实施例3：
成分：0.775Bi1.05FeO3-0.025BiAlO3+0.20Bi(Ti0.5Zn0.5)O3+0.01Ba(W0.5Cu0.5)O3+0.01Li2CO3+0.01MnCO3，以分析纯Fe2O3、Bi2O3、TiO2、ZnO、BaCO3、Al2O3、W2O3、CuO、Li2CO3、MnCO3为原料，制备方法同实施例1，烧结温度为970℃。
性能测量结果如下：
d<sub>33</sub>(pC/N) Q<sub>m</sub> k<sub>p</sub>(％) ε<sub>r</sub> Tc(℃) T<sub>d</sub>(℃)
15 67.4 0.29 119 675 645
实施例4：
成分：0.7Bi1.05FeO3-0.05BiAlO3+0.2Bi(Ti0.5Zn0.5)O3+0.01CuO+0.01MnCO3，以分析纯Fe2O3、Bi2O3、TiO2、ZnO、Al2O3、CuO、MnCO3为原料，制备方法同实施例1，不同的是烧结温度为1020℃。
性能测量结果如下：
d<sub>33</sub>(pC/N) Q<sub>m</sub> k<sub>p</sub>(％) ε<sub>r</sub> Tc(℃) T<sub>d</sub>(℃)
13 47.9 0.22 99.4 670 635
本发明所列举的成分的上下限、区间取值以及工艺参数的上下限、区间取值都能实现本发明，在此不一一列举实施。

Claims (2)

1.一种具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷，其特征在于，其组成通式为：xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3，其中x、y、z、t、m表示摩尔分数，P为Ba(W0.5Cu0.5)O3、CuO、Li2CO3中的一种或多种烧结助剂的组合，且0.5≤x≤0.8,0<y≤0.10,0<z≤0.20,0<t≤0.1,0<m≤0.1。
2.权利要求书1所述的具有零温度系数及高温稳定性的铁酸铋-铝酸铋-锌钛酸铋高温压电陶瓷的制备方法，其特征在于，包括如下步骤：
(1)以分析纯Fe2O3、Bi2O3、TiO2、ZnO、BaCO3、Al2O3、W2O3、CuO、MnCO3、Li2CO3为原料，按照xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3进行配料，其中0.5≤x≤0.8,0<y≤0.10,0<z≤0.20,0<t≤0.1,0<m≤0.1，P为Ba(W0.5Cu0.5)O3、CuO、Li2CO3中的一种或多种烧结助剂的组合，将混合粉末以无水乙醇为介质球磨24小时，100℃/12小时在烘箱中烘干、过筛，放入高铝坩埚中压实加盖，再放入密闭管式炉中通纯氧气以250℃/h的升温速率到850℃预烧，保温6小时合成，并降温冷却至200℃以下后取出备用；
(2)将步骤(1)合成的xBi1.05FeO3-yBiAlO3+zBi(Ti0.5Zn0.5)O3+tP+mMnCO3粉末以无水乙醇为介质进行二次球磨24小时，取出干燥，过筛；
(3)将过筛后的粉末加入质量百分比浓度为5％PVA的溶液造粒，在钢模中于100MPa下压制成型，模具内直径为1cm；
(4)成型的素片放入马弗炉中以30℃/h的升温速率缓慢升温至600℃，保温24小时排胶；然后以20℃/min的升温速率快速升温到980-1020℃，保温120分钟后随炉冷却至室温；
(5)将烧结后样品抛光成两面光滑、厚度1mm的薄片，披银电极，650℃/30分钟烧银后备用；
(6)将披银电极后的压电陶瓷片在硅油中极化，极化电场6000V/mm，极化温度150℃，时间30分钟，保持电场冷却至室温。
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