CN112457011A - 扬声器用四元系压电陶瓷及其制备方法 - Google Patents
扬声器用四元系压电陶瓷及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000007873 sieving Methods 0.000 claims abstract description 15
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- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 12
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- 238000000034 method Methods 0.000 claims description 9
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
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- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了一种扬声器用四元系压电陶瓷及其制备方法。其压电陶瓷的材料组成化学式为Pb(Sn0.5Nb0.5)O3‑Pb(Ni1/3Nb2/3)O3‑Pb[ZrxTi(1‑x)]O3，其中x=0.4‑0.45，选用0.05wt.%‑3.5 wt.%的CeO2进行掺杂改性。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800℃预烧4h，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1280℃、保温2h得陶瓷片，陶瓷片上电极，并温度为于75℃、电场强度为2.3KV/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500‑580左右，压电陶瓷材料的介电常数为2000‑3000。
Description
技术领域
本发明涉及一种压电陶瓷及其制备方法，尤其涉及一种扬声器用四元系压电陶瓷及其制备方法；具体涉及一种PSN-PNN-PZT压电陶瓷及其制备方法。
背景技术
随着现代电子信息产业的蓬勃发展，压电陶瓷元器件在微机电系统压电致动器、传感器、蜂鸣器以及扬声器等设备上被大规模应用。相较于传统电磁扬声器，压电扬声器利用逆电效应的原理将声信号和电信号进行相互转化，它具有尺寸小、质量轻、功耗低、抗电磁干扰能力强以及安全可靠性高等一系列优点。
目前，国内已率先在手机微型扬声器上大规模地采用了压电陶瓷元器件。Pb(Ni1/ 3Nb2/3)O3-Pb(ZrxTi1-x)O3(PNN-PZT)三元系压电陶瓷因其优良的压电特性、低成本及高的机械品质因数已成为最理想的压电材料。然而总的来说，PNN-PZT三元系压电陶瓷属于典型的软性掺杂材料，存在介电常数小、低居里温度（约120oC）等不足。通常的音频元器件需要较高的介电常数，因此选择合适的成分配方，优化制备工艺，拟获得优异的电学性能相配合的压电陶瓷材料是压电扬声器发展所需解决的关键问题。
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扬声器用四元系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，本发明提供的扬声器用四元系压电陶瓷的材料组成化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，其中x=0.4-0.45，选用0.05wt.% - 3.5wt.%的CeO2进行掺杂改性。
为了制备上述扬声器用四元系压电陶瓷，本发明提供的制备方法如下：
1）按照权利要求1中的化学式秤取Pb3O4、ZrO2、TiO2、Nb2O5、SnO2、Ni2O3、CeO2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800℃，保温4h，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1280℃，保温2h，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2.3KV/mm的硅油中极化20min，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，本发明采用上述技术方案，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500-580；压电陶瓷材料的介电常数为2000-3000。
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；其次本发明所制备压电陶瓷材料尺寸小、相对介电常数高、综合压电性能好，是良好的压电扬声器用陶瓷材料；最后，适量的CeO2掺杂可有效提高压电陶瓷的综合电学性能，使之更好的匹配扬声器的性能要求。
附图说明
图1是不同Ce含量掺杂PSN-PNN-PZT压电陶瓷的XRD图谱；
图2是0.2%Ce含量掺杂PSN-PNN-PZT压电陶瓷的断面SEM图片；
图3是0.35%Ce含量掺杂PSN-PNN-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Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.05wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，具体步骤如下：
1）根据上述化学式秤取Pb3O4、ZrO2、TiO2、Nb2O5、SnO2、Ni2O3、CeO2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800℃，保温4h，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1280℃，保温2h，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2.3KV/mm的硅油中极化20min，得压电陶瓷片。
实施例2
制备化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.10wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，各步骤同实施例1。
实施例3
制备化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.15wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，各步骤同实施例1。
实施例4
制备化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.20wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，各步骤同实施例1。
实施例5
制备化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.25wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，各步骤同实施例1。
实施例6
制备化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.30wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，各步骤同实施例1。
实施例7
制备化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，x=0.4-0.45，选用0.35wt.%的CeO2进行掺杂改性的扬声器用四元系压电陶瓷，各步骤同实施例1。
以下是上述各实施例制备的扬声器用四元系压电陶瓷的电性能测试结果。
表1：不同Ce含量掺杂PSN-PNN-PZT压电陶瓷的电学性能
| 掺杂铈含量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 | 0.012 | 0.596 | 527 | 2465 |
| 0.10 | 0.016 | 0.616 | 563 | 3223 |
| 0.15 | 0.017 | 0.623 | 583 | 3310 |
| 0.20 | 0.0168 | 0.621 | 585 | 3324 |
| 0.25 | 0.0163 | 0.597 | 511 | 3081 |
| 0.30 | 0.0171 | 0.605 | 529 | 2952 |
| 0.35 | 0.017 | 0.584 | 558 | 3098 |
由表1可知，掺杂前，压电陶瓷机电耦合系数kp、压电常数d 33和介电常数ε r值均较低。而当CeO2掺杂量为0.15和0.20wt.%时，压电陶瓷的机电耦合系数kp、压电常数d 33和介电常数ε r值均达到最大值，电性能最优。而随着CeO2含量进一步增加，陶瓷的压电性能、机电耦合系数、介电常数均有显著下降。
从图1可以看出，掺杂前，PSN-PNN-PZT压电陶瓷的相结构为单一钙钛矿结构；而掺杂少量CeO2稀土氧化物后，陶瓷的相结构并未发生明显变化，仍为单一钙钛矿结构。可见，Ce4+完全充分固溶入钙钛矿晶格内部，并未在晶间区域形成其它物相。
图2-3为不同铈含量掺杂PSN-PNN-PZT压电陶瓷的断面SEM图片。从图中可以看出，经1280℃烧结2h后，各压电陶瓷样品显微组织均匀，晶粒大小一致，但0.35wt% CeO2掺杂后的陶瓷内部存在明显的孔洞缺陷，陶瓷致密度较差。该现象表明合适的CeO2掺杂量可有效提高陶瓷的致密度。
Claims (3)
1.一种扬声器用四元系压电陶瓷，其特征在于：压电陶瓷的材料组成化学式为Pb(Sn0.5Nb0.5)O3-Pb(Ni1/3Nb2/3)O3-Pb[ZrxTi(1-x)]O3，其中x=0.4-0.45，选用0.05wt.% - 3.5wt.%的CeO2进行掺杂改性。
2.一种实现权利要求1所述的扬声器用四元系压电陶瓷制备方法，其特征在于：
1）按照权利要求1中的化学式秤取Pb3O4、ZrO2、TiO2、Nb2O5、SnO2、Ni2O3、CeO2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800℃，保温4h，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1280℃，保温2h，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2.3KV/mm的硅油中极化20min，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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