CN112430088A - 压电报警器用压电陶瓷及其制备方法 - Google Patents

压电报警器用压电陶瓷及其制备方法 Download PDF

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CN112430088A
CN112430088A CN202011457965.5A CN202011457965A CN112430088A CN 112430088 A CN112430088 A CN 112430088A CN 202011457965 A CN202011457965 A CN 202011457965A CN 112430088 A CN112430088 A CN 112430088A
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ceramic
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张静
江平
张元松
褚涛
王渝
钟敏
官瑶
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Guizhou Zhenhua Hongyun Electronics Co ltd
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Abstract

本发明公开了一种压电报警器用压电陶瓷及其制备方法。其压电陶瓷的材料组成化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.05wt%，x=0.15wt%，x=0.2wt%，x=0.25wt%，x=0.3wt%，x=0.35wt%。其制备方法是将化学式中的粉体混合后进行一次湿法球磨4h，烘干过筛后1000℃预烧2h，然后再进行二次湿法球磨4h，烘干过筛后加入8%的聚乙烯醇水溶液，造粒、过筛、压制成坯体，坯体在600℃下排胶2h后升温至1250℃、保温4h得陶瓷片，陶瓷片上电极，并温度为于75℃、电场强度为3KV/mm的硅油中极化25min，得压电陶瓷片。本发明压电陶瓷的压电性能d 33为600左右，压电陶瓷材料的介电常数为2000‑2500。

Description

压电报警器用压电陶瓷及其制备方法
技术领域
本发明涉及一种压电陶瓷及其制备方法，尤其涉及一种压电报警器用压电陶瓷及其制备方法；具体涉及一种PZT-PSN压电陶瓷及其制备方法。
背景技术
压电陶瓷属于多晶型具有较强压电效应的陶瓷材料，其内部晶粒多为可自发极化的电畴，这些电畴的方向原本为随机排列，但在外加电场作用下可使其呈规则排列，从而表现出压电特性。作为一种重要的力-电转换材料，压电陶瓷报警器因其低成本、尺寸小、能耗低和可靠性高等优势已被大规模工业应用。
压电报警器是压电陶瓷一个新兴的应用方向，它是以压电陶瓷为高分贝振动源的报警类电子元器件。目前，压电报警器已被广泛应用在家用洗衣机、电子锁及微波炉等家用电器内。不同于普通蜂鸣器件，压电报警器应具有高声压、高安全指数及优良的可靠性，这对压电陶瓷提出了更高的电性能要求。通常，报警器用压电陶瓷的压电常数d 33不低于600pC / N，机械品质因数应高于65%，相对介电常数应不低于2500，介电损耗低于3%。PZT压电陶瓷由于良好的压电性能、高的机电耦合系数和优异的机械品质因数等均远远优于其它体系压电陶瓷材料(钛酸钡、铌酸钠钾等)，因此，目前市场上所使用的压电材料绝大多数为PZT体系陶瓷。本发明拟在Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3压电陶瓷的基础上，利用微量MnO2进行掺杂改性，以获得高压电常数和介电常数的报警器用压电陶瓷材料。
发明内容
针对现有技术存在的上述缺陷，本发明旨在提供一种压电报警器用压电陶瓷及其制备方法，以获得高压电常数和介电常数。
为了实现上述目的，本发明提供的压电报警器用压电陶瓷的材料组成化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，其中x=0.05wt%，x=0.15wt%，x=0.2wt%，x=0.25wt%，x=0.3wt%，x=0.35wt%。
为了制备所述压电报警器用压电陶瓷，本发明提供的制备方法如下：
1）按照上述化学式秤取Pb3O4、ZrO2、TiO2、Nb2O5、Sb2O3、MnO2、SrCO3粉体，将各粉体混合后得一次磨料；
2）按2:1:1的质量比将水、所述一次磨料、磨球混合，球磨4h后烘干、过筛；
3）将筛下物送入烧结炉中，按3℃/min的速率升温至1000℃，保温2h，冷却后过筛，得二次磨料；
4）按2:1:1的质量比将水、所述二次磨料、磨球混合，球磨4h后烘干、过筛，得陶瓷粉体；
5）向所述陶瓷粉体中加入质量分数百分比为8%的聚乙烯醇水溶液，混匀、造粒、过筛、压制成型，得陶瓷片坯体；
6）将所述陶瓷片坯体送入烧结炉中，600℃下排胶2h，然后按1.5℃/min的速率升温至1250℃，保温4h，得到陶瓷片；
7）在所述陶瓷片上印刷银电极，烘干后将其送入烧结炉中并按3℃/min的速率升温至850℃，然后随炉冷却
8）将经过烧银处理的陶瓷片置于温度为75℃、电场强度为3KV/mm的硅油中极化25min，得压电陶瓷片。
在上述步骤中，所述磨球为锆球，所述水为去离子水。
与现有技术比较，本发明由于采用了上述技术方案，因此具有以下优点：
1、制备出了压电陶瓷材料的压电性能d 33达600；压电陶瓷材料的介电常数为2000~2500。
2、本发明的制备方法简单，对设备无特殊需求，成本低，适合大规模生产，符合工业需求。
3、与现有技术相比，本发明所用原材料均为价格低廉的非金属氧化物，制作工艺为传统固相烧结，成本较低，利于大规模工业生产应用；其次，适量的MnO2掺杂可有效提高压电陶瓷的综合电学性能，使之更好的匹配报警器的性能要求。最后，本发明所制备压电陶瓷材料尺寸小、综合压电性能好，能较好满足压电报警器的性能要求，是理想的压电报警器用陶瓷材料。
附图说明
图1是不同Mn含量掺杂PSN-PZT压电陶瓷的XRD图谱；
图2是0.05%锰含量掺杂PSN-PZT压电陶瓷的断面SEM图片；
图3是0.15%锰含量掺杂PSN-PZT压电陶瓷的断面SEM图片；
图4是0.30%锰含量掺杂PSN-PZT压电陶瓷的断面SEM图片。
具体实施方式
下面结合附图和具体的实施例对本发明作进一步说明。
实施例1
制备化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.05wt% 的压电报警器用陶瓷，具体步骤如下：
1）根据上述化学式秤取Pb3O4、ZrO2、TiO2、Nb2O5、Sb2O3、MnO2、SrCO3粉体的质量wt%数，将各粉体混合后得一次磨料；
2）按2:1:1的质量比将去离子水、所述一次磨料、锆球混合，以300 r/min的转速球磨4h，再于70℃的真空环境中干燥3h，过40目筛；
3）将筛下物送入烧结炉中，按3℃/min的速率升温至1000℃，保温2h，冷却后过40目筛，得二次磨料；
4）按2:1:1的质量比将去离子水、所述二次磨料、锆球混合，以300 r/min的转速球磨4h，再于70℃的真空环境中干燥3h，过40目筛，得陶瓷粉体；
5）向所述陶瓷粉体中加入质量分数百分比为8%的聚乙烯醇水溶液，混匀、造粒、过筛，在12Mp下压制成Φ10×1mm的陶瓷片坯体；
6）将所述陶瓷片坯体送入烧结炉中，600℃下排胶2h，然后按1.5℃/min的速率升温至1250℃，保温4h，得到陶瓷片；
7）在所述陶瓷片上印刷银电极，烘干后将其送入烧结炉中并按3℃/min的速率升温至850℃，然后随炉冷却
8）将经过烧银处理的陶瓷片置于温度为75℃、电场强度为3KV/mm的硅油中极化25min，得压电陶瓷片。
实施例2
制备化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.15wt% 的压电报警器用陶瓷，各步骤同实施例1。
实施例3
制备化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.20wt% 的压电报警器用陶瓷，各步骤同实施例1。
实施例4
制备化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.25wt% 的压电报警器用陶瓷，各步骤同实施例1。
实施例5
制备化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.30wt% 的压电报警器用陶瓷，各步骤同实施例1。
实施例6
制备化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，x=0.35wt% 的压电报警器用陶瓷，各步骤同实施例1。
以下是上述各实施例制备的压电报警器用陶瓷的电性能测试结果。
表1：不同Mn含量掺杂PZT-PSN压电陶瓷的电学性能
掺杂锰含量wt.% <i>tgδ</i> <i>k</i><sub>p</sub> <i>d</i><sub>33 </sub>pC/N <i>ε</i><sub>r</sub>
0.05% 0.0083 0.625 532 2194
0.15% 0.0095 0.654 611 2523
0.20% 0.0062 0.559 454 1475
0.25% 0.0069 0.499 380 1246
0.30% 0.0075 0.516 411 1758
0.35% 0.0079 0.519 370 1984
由表1可知，当Mn掺杂量为0.15 wt.%时，压电陶瓷表现出最优的综合电学性能：tgδ=0.95%远低于3%，kp=0.654略高于65%，d 33=611 pC/N略高于600 pC/N，ε r刚好满足报警器的性能要求。但随着MnO2含量过高时，压电陶瓷的电学性能显著下降。
从图1可以看出，所有衍射峰均对应钙钛矿结构的标准谱。图中衍射最强的是四方峰，材料主要由四方相组成。在2θ=22°，32°，38°，50°和55°附近衍射峰发生明显的***，表明三方相和四方相共存。其中谱线1为少量掺杂的陶瓷的XRD线，可以看出基础配方的锆钛比在50：50与52：48之间。谱线2为掺杂0.15%的XRD线，其锆钛比更接近于52：48，此时材料处于准同型相界，其性能也更好，如表1。然而，随着锰含量的增加，锆钛比越来越偏离52：48，各项性能也随之降低。
图2-4为不同锰含量掺杂PSN-PZT压电陶瓷的断面SEM图片。从图中可以看出，锰有促进陶瓷晶粒长大的作用。随着锰含量的增加，晶粒越来越致密，当锰含量超过0.2%时锰的作用不再明显。当锰含量为0.15%时，晶粒生长很好，瓷体的致密度最高，气孔小，气孔率低。这是因为适量的锰固熔到晶格内部，降低晶粒界面能和晶粒生长的推动力，促进晶粒的生长。但是超过了0.2%，陶瓷无明显的晶界，气孔率高。这是过量的锰集聚在晶界的位置，严重影响陶瓷的性能。可以得出，与基础配方相比，掺杂0.15%的锰，晶粒生长很好，瓷体的致密度最高、气孔小、气孔率低，陶瓷各项性能较高。

Claims (3)

1.一种压电报警器用陶瓷，其特征在于：该压电报警器压电陶瓷的材料组成化学式为Pb0.98Sr0.02(Zr53Ti47)0.9(Sb1/3Nb2/3)0.1O3+x MnO2，其中x=0.05wt%，x=0.15wt%，x=0.2wt%，x=0.25wt%，x=0.3wt%，x=0.35wt%。
2.一种实现权利要求1所述的压电报警器用陶瓷制备方法，其特征在于：
1）按照权利要求1中的化学式秤取Pb3O4、ZrO2、TiO2、Nb2O5、Sb2O3、MnO2、SrCO3粉体，将各粉体混合后得一次磨料；
2）按2:1:1的质量比将水、所述一次磨料、磨球混合，球磨4h后烘干、过筛；
3）将筛下物送入烧结炉中，按3℃/min的速率升温至1000℃，保温2h，冷却后过筛，得二次磨料；
4）按2:1:1的质量比将水、所述二次磨料、磨球混合，球磨4h后烘干、过筛，得陶瓷粉体；
5）向所述陶瓷粉体中加入质量分数百分比为8%的聚乙烯醇水溶液，混匀、造粒、过筛、压制成型，得陶瓷片坯体；
6）将所述陶瓷片坯体送入烧结炉中，600℃下排胶2h，然后按1.5℃/min的速率升温至1250℃，保温4h，得到陶瓷片；
7）在所述陶瓷片上印刷银电极，烘干后将其送入烧结炉中并按3℃/min的速率升温至850℃，然后随炉冷却
8）将经过烧银处理的陶瓷片置于温度为75℃、电场强度为3KV/mm的硅油中极化25min，得压电陶瓷片。
3.根据权利要求2所述的压电报警器用陶瓷制备方法，其特征在于：所述磨球为锆球，所述水为去离子水。
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