CN110498679A - 一种高介电性能多层相结构bnt-bt陶瓷的制备方法 - Google Patents

一种高介电性能多层相结构bnt-bt陶瓷的制备方法 Download PDF

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CN110498679A
CN110498679A CN201910924240.3A CN201910924240A CN110498679A CN 110498679 A CN110498679 A CN 110498679A CN 201910924240 A CN201910924240 A CN 201910924240A CN 110498679 A CN110498679 A CN 110498679A
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王军军
柏春庚
吴丰民
林炜鹏
张春晓
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Harbin University of Science and Technology
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Abstract

一种高介电性能多层相结构BNT‑BT陶瓷的制备方法，属于压电陶瓷的技术领域。本发明要现有解决BNT‑BT陶瓷的介点性能较低的技术问题。本发明方法：步骤1、制备三方相BNT‑5BT粉料、准同型相界BNT‑7BT粉料四方向相BNT‑9BT粉料；步骤2、将步骤1得到的四方相BNT‑9BT粉料放入模具中，压制成型，再放入步骤1得到的准同型相界BNT‑7BT粉料后，压制成型，然后放入步骤1得到的三方相BNT‑5BT粉料，压制成型；步骤3、然后高压成型，烧结，随炉自然冷却，得到多层相结构BNT‑BT陶瓷。本发明制备出无分层，组分之间相互固溶的类三明治结构陶瓷，从而提高其介电性能。

Description

一种高介电性能多层相结构BNT-BT陶瓷的制备方法
技术领域
本发明属于压电陶瓷的技术领域；具体涉及一种高介电性能多层相结构BNT-BT陶瓷的制备方法。
背景技术
压电陶瓷是一种应用广泛的功能性材料，被广泛应用于超声换能、无损探伤、传感器、电子信息等高新技术领域，涉及汽车、电子、军事、医疗等各个行业。现阶段最常用的是PZT等含铅陶瓷，PZT系压电陶瓷具有十分优异的压电性能，并且通过掺杂改性可以满足许多不同的性能要求，因而广受欢迎。但由于含铅陶瓷在制备和回收过程中，铅的挥发对人类和自然环境造成危害，为了可持续发展，无铅压电陶瓷的研究和开发是当前压电铁电材料领域的研究热点之一。
钛酸铋钠(sodiumbismuth titanate，BNT)基无铅压电陶瓷，通过与其他铁电体系进行固溶，如钛酸钡(barium titanate，BT)，进行固溶之后形成二元固溶体系钛酸铋钠-钛酸钡((1-x％)(Bi0.5Na0.5)TiO3-x％BaTiO3，BNT-xBT)根据组分的不同当x＝5时为三方相，x＝7处于准同型相界组分，当x＝9时为四方相。
BNT-BT陶瓷由于具有较好的压电性能(约为125pC/N)和较好的声学性能等等优点，一直被认为是PZT的替代品之一。但是它也有一系列的缺点：它的介点性能较低(x＝7时准同相界约为580)。
发明内容
本发明要现有解决BNT-BT陶瓷的介点性能较低的技术问题；而提供了一种高介电性能多层相结构BNT-BT陶瓷的制备方法。
为解决上述技术问题，本发明中一种高介电性能多层相结构BNT-BT陶瓷的制备方法是按下述步骤进行的：
步骤1、按照(1-0.05)(Bi0.5Na0.5)TiO3-0.05BaTiO3化学计量比，分别称取Bi2O3(质量纯度≥99％)、Na2CO3(质量纯度≥99.5％)、BaCO3(质量纯度≥99％)、TiO2(质量纯度≥99.9％)，混匀，得到BNT-5BT原料粉，再按照(1-0.07)(Bi0.5Na0.5)TiO3-0.07BaTiO3化学计量比，分别称取Bi2O3(质量纯度≥99％)、Na2CO3(质量纯度≥99.5％)、BaCO3(质量纯度≥99％)、TiO2(质量纯度≥99.9％)，得到BNT-7BT原料粉，再按照(1-0.09)(Bi0.5Na0.5)TiO3-0.09BaTiO3化学计量比，分别称取Bi2O3(质量纯度≥99％)、Na2CO3(质量纯度≥99.5％)、BaCO3(质量纯度≥99％)、TiO2(质量纯度≥99.9％)，得到BNT-9BT原料粉，然后对BNT-5BT原料粉、BNT-7BT原料粉、BNT-9BT原料粉进行下述操作：
步骤1.1将原料粉采用无水乙醇作为分散剂进行球磨12h～24h，
步骤1.2然后在90℃～120℃下烘干后研磨，压片，在800℃～850℃下预烧4h～6h，
步骤1.3然后压碎后研磨，加入无水乙醇进行二次球磨12h～24h，
步骤1.4在90℃～120℃下烘干，再加入PVA后研磨至均匀，在干燥环境下静置至少12h，然后筛取100目～160目之间的粉末，分别得到三方相BNT-5BT粉料、准同型相界BNT-7BT粉料四方相BNT-9BT粉料；
步骤2、将步骤1得到的四方相BNT-9BT粉料放入模具中，压制成型，再放入步骤1得到的准同型相界BNT-7BT粉料后，压制成型，然后放入步骤1得到的三方相BNT-5BT粉料，压制成型；
步骤3、然后在压强为8Mpa～10Mpa、时间为4min～6min下进行高压成型，然后以4℃/min速率升温，在1150℃条件下进行烧结2h～3h，随炉冷却，得到多层相结构BNT-BT陶瓷。
进一步限定，步骤1.1中研磨时间16h。
进一步限定，步骤1.3中研磨时间20h。
进一步限定，步骤1.4中PVA用量是步骤二烘干后混合粉体的3％wt～5％wt。
进一步限定，四方相BNT-9BT粉料、准同型相界BNT-7BT粉料与三方相BNT-5BT质量比为(0.3～0.5)：(0.3～0.5)：(0.3～0.5)。
本发明制备出无分层，组分之间相互固溶的类三明治结构陶瓷，从而提高其介电性能。
附图说明
图1是烧结后陶瓷样品：a)陶瓷烧结样品，b)陶瓷切割面图；
图2是不同电场下陶瓷铁电电滞回线图；
图3是陶瓷电滞回线和漏电图；
图4是不同频率下陶瓷介电常数-温度曲线图。
具体实施方式
实施例1：本实施例中一种高介电性能多层相结构BNT-BT陶瓷的制备方法是按下述步骤进行的：
步骤1、按照(1-0.05)(Bi0.5Na0.5)TiO3-0.05BaTiO3化学计量比，分别称取Bi2O3(质量纯度99％)、Na2CO3(质量纯度99.5％)、BaCO3(质量纯度99％)、TiO2(质量纯度99.9％)，混匀，得到BNT-5BT原料粉，再按照(1-0.07)(Bi0.5Na0.5)TiO3-0.07BaTiO3化学计量比，分别称取Bi2O3(质量纯度99％)、Na2CO3(质量纯度99.5％)、BaCO3(质量纯度99％)、TiO2(质量纯度99.9％)，混匀，得到BNT-7BT原料粉，再按照(1-0.09)(Bi0.5Na0.5)TiO3-0.09BaTiO3化学计量比，分别称取Bi2O3(质量纯度99％)、Na2CO3(质量纯度99.5％)、BaCO3(质量纯度99％)、TiO2(质量纯度99.9％)，混匀，得到BNT-9BT原料粉，然后对BNT-5BT原料粉、BNT-7BT原料粉、BNT-7BT原料粉进行下述操作：
步骤1.1将原料粉采用无水乙醇作为分散剂进行球磨16h，
步骤1.2然后在90℃下烘干4h后研磨0.5h，压片，在800℃下预烧4h；
步骤1.3然后压碎后研磨0.5h，加入无水乙醇进行二次球磨12h，
步骤1.4在90℃下烘干，再加入5％wt PVA后研磨至均匀，在干燥环境下静置12h，然后筛取100目～160目之间的粉末，分别得到三方相BNT-5BT粉料、准同型相界BNT-7BT粉料四方相BNT-9BT粉料；
步骤2、将0.3g步骤1得到的四方相BNT-9BT粉料放入模具中，压制成型，再放入0.3g步骤1得到的准同型相界BNT-7BT粉料后，压制成型，然后放入0.3g步骤1得到的三方相BNT-5BT粉料，压制成型；
步骤3、然后在压强为8Mpa、时间为4min下进行高压成型直径为13mm圆片，然后以4℃/min速率升温，在1150℃条件下进行烧结3h，随炉冷却，得到多层相结构BNT-BT陶瓷。
烧结后多层相结构BNT-BT陶瓷样品如图1所示，收缩均匀，无分层，得到质量良好的陶瓷样品；图2可以看出，随着测试电场强度的增大，电滞回线逐渐趋于饱和，剩余极化强度及矫顽场随之增加；图3中给出了漏电流随电场强度的变化曲线，可以看出，在矫顽场位置漏电流有突然增大的现象，表明压电陶瓷的绝大部分电畴在此电场强度下发生翻转；此外，正负方向矫顽场位置对应的漏电流不同，负方向矫顽场对应的漏电流为-0.66mA/cm2，正方向矫顽场对应的漏电流为0.48mA/cm2，这是由于上下层分别为三方相、四方相结构，电畴结构不同，产生的漏电流也有差异造成的结果；图4为复合结构陶瓷极化后的介温图谱，存在三个介电突变峰，分别为退极化温度Td、三方-四方铁电相变温度TO-T和介电常数最大值温度Tm，分别为：Td＝148℃，TO-T＝189℃，Tm＝293℃.室温下，复合结构陶瓷极化前相对介电系数(εr/ε0)为1278，极化后相对介电系数(ε33/ε0)为808，同准同型相界组分BNT-BT陶瓷相比，介电性能有明显的提高。

Claims (8)

1.一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于所述多层相结构BNT-BT陶瓷的制备方法是按下述步骤进行的：
步骤1、按照(1-0.05)(Bi0.5Na0.5)TiO3-0.05BaTiO3化学计量比，分别称取Bi2O3、Na2CO3、BaCO3、TiO2，混匀，得到BNT-5BT原料粉，再按照(1-0.07)(Bi0.5Na0.5)TiO3-0.07BaTiO3化学计量比，分别称取Bi2O3、Na2CO3、BaCO3、TiO2，混匀，得到BNT-7BT原料粉，再按照(1-0.09)(Bi0.5Na0.5)TiO3-0.09BaTiO3化学计量比，分别称取Bi2O3、Na2CO3、BaCO3、TiO2，混匀，得到BNT-9BT原料粉，然后对BNT-5BT原料粉、BNT-7BT原料粉、BNT-7BT原料粉进行下述操作：
步骤1.1将原料粉采用无水乙醇作为分散剂进行球磨12h～24h，
步骤1.2然后在90℃～120℃下烘干后研磨，压片，在800℃～850℃下预烧4～6h，
步骤1.3然后压碎后研磨，加入无水乙醇进行二次球磨12h～24h，
步骤1.4在90℃～120℃下烘干，再加入PVA后研磨至均匀，在干燥环境下静置至少12h，然后筛取100目～160目之间的粉末，分别得到三方相BNT-5BT粉料、准同型相界BNT-7BT粉料四方相BNT-9BT粉料；
步骤2、将步骤1得到的四方相BNT-9BT粉料放入模具中，压制成型，再放入步骤1得到的准同型相界BNT-7BT粉料后，压制成型，然后放入步骤1得到的三方相BNT-5BT粉料，压制成型；
步骤3、然后在压强为8Mpa～10Mpa、时间为4min～6min下进行高压成型，然后以4℃/min速率升温，在1150℃条件下进行烧结2h～3h，随炉冷却，得到多层相结构BNT-BT陶瓷；
其中，步骤一中Bi2O3的质量纯度≥99％，Na2CO的质量纯度≥99.5％，BaCO3的质量纯度≥99％，TiO2的质量纯度≥99.9％。
2.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤1.1中研磨时间16h。
3.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤1.3中研磨时间20h。
4.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤1.2中在800℃下预烧4h。
5.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤1.4中PVA用量是步骤二烘干后混合粉体的3％wt～5％wt。
6.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤2中四方相BNT-9BT粉料、准同型相界BNT-7BT粉料与三方相BNT-5BT质量比为(0.3～0.5g)：(0.3～0.5g)：(0.3～0.5g)。
7.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤3中在压强8Mpa、时间为4min下进行高压成型。
8.根据权利要求1所述一种高介电性能多层相结构BNT-BT陶瓷的制备方法，其特征在于步骤3中在1150℃条件下进行烧结3h。
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