CN112047734B - 一种屏幕发声用压电陶瓷及制备方法 - Google Patents
一种屏幕发声用压电陶瓷及制备方法 Download PDFInfo
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Abstract
本发明公开了一种屏幕发声用压电陶瓷,包括以下列化学式I表示:(1‑y)(0.65Pb(Zr1‑xTix)O3‑0.35Pb(Ni0.33M0.67)O3)‑yCa1.9Ba0.1Nb2O7+zCuO,所述M选自Nb、Ta和Sb中的任意一种,所述x、y和z均表示摩尔百分比,z为CuO所占化合物(1‑y)(0.65Pb(Zr1‑xTix)O3‑0.35Pb(Ni0.33M0.67)O3)‑yCa1.9Ba0.1Nb2O7的摩尔百分比的数值,其中0.4<x<0.7,0.01<y<0.25,0<z<0.04本发明涉及压电陶瓷技术领域。该屏幕发声用压电陶瓷的制备方法,S1、配料:S2、制备:S21、合成:S22、造粒:S23、压制:S24、排胶:S25、烧结:S3、极化:S31、将陶瓷元件进行极化,以得到压电陶瓷。
Description
技术领域
本发明涉及压电陶瓷技术领域,具体为一种屏幕发声用压电陶瓷及制备方法。
背景技术
智能手机正在向全面屏以及无孔化的方向发展,因此屏幕发声激励器广受关注。相比于传统受话器以及扬声器,使用屏幕发声激励器,无需开孔,可以简化工艺流程以及降低成本,并且提升手机美观度。目前有两种屏幕发声技术,一种是基于电磁振动原理,另外一种是基于压电效应。由于具有厚度小、功耗低、无电磁干扰以及对音腔要求低等优点,压电式屏幕发声技术应用前景佳。
压电式屏幕发声激励器核心元件是多层压电陶瓷,所使用的压电陶瓷材料特性将直接影响激励器的最终电声性能。目前市场上主要使用低温烧结的PZT-5H系列压电陶瓷来制作激励器。PZT-5H系列压电陶瓷具有较高的压电系数d33和机械耦合系数Kp,但是居里温度Tc较低,另外,其烧结温度一般低于950℃,这样可以在制备多层陶瓷时可以使用价格较低的纯Ag作为内电极,从而降低器件的整体成本。
在智能手机组装和生产过程中,需要进行回流焊工艺,所涉及的最高温度超过250℃,同时也超过PZT-5H系列压电陶瓷的居里温度,因此压电陶瓷容易发生退极化,从而使激励器发生失效,而目前这一问题并没有得到很好的解决。因此针对屏幕发声应用,迫切需要开发一种兼具高压电性能、低烧结温度以及高居里温度的新型压电陶瓷材料。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种屏幕发声用压电陶瓷及制备方法,解决了在智能手机组装和生产过程中,需要进行回流焊工艺,所涉及的最高温度超过250℃,同时也超过PZT-5H系列压电陶瓷的居里温度,因此压电陶瓷容易发生退极化,从而使激励器发生失效的问题。
(二)技术方案
为实现以上目的,本发明通过以下技术方案予以实现:一种屏幕发声用压电陶瓷,包括以下列化学式I表示:(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7+zCuO,其特征在于:所述M选自Nb、Ta和Sb中的任意一种,所述x、y和z均表示摩尔百分比,所述z为CuO所占化合物(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7的摩尔百分比的数值,其中0.4<x<0.7,0.01<y<0.25,0<z<0.04。
优选的,所述x、y和z,其中0.47≤x≤0.62,0.02≤y≤0.18,0.01≤z≤0.03。
优选的,所述M为Nb。
优选的,所述压电陶瓷处于三方和四方相共存状态。
本发明还公布一种屏幕发声用压电陶瓷的制备方法,具体包括如下步骤:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料
各种原料根据化学式(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y和z均表示摩尔百分比,
其中0.4<x<0.7,0.01<y<0.25。
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3和BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷。
优选的,所述S21步骤中,合成温度为700-900℃,保温时间为2-4h。
优选的,所述S22步骤中,粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为3%-10%。
优选的,所述S25步骤中,烧结温度为900-950℃,保温时间为2-6h。
优选的,所述S3步骤中,在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为400-700℃,保温时间为1-3h。
优选的,所述S3步骤中,所述极化的温度为80-140℃,极化电压为2-5kV/mm。
(三)有益效果
本发明提供了一种屏幕发声用压电陶瓷及制备方法。与现有技术相比具备以下有益效果:
该屏幕发声用压电陶瓷及制备方法,针对目前压电式屏幕发声激励器所使用的高性能压电陶瓷材料居里温度低,在回流焊过程中容易发生退极化的技术问题,本发明提出了一种新的技术方案,通过在0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3(M选自Nb、Ta和Sb中的任意一种)中引入具有超高居里温度和层状钙钛矿结构的Ca1.9Ba0.1Nb2O7,从而形成固溶体,并在其中掺入适量的CuO来作为低温烧结助剂,可以获得兼具高压电性能、低烧结温度以及高居里温度的新型压电陶瓷材料,从而有效的解决这一问题。
具体实施方式
对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明实施例提供五种技术方案:
方案1:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料
各种原料根据化学式
(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y和z均表示摩尔百分比,
其中x=0.5,y=0.15,z=0.01。
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3和BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;合成温度为700℃,保温时间为2h;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为3%;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;烧结温度为900℃,保温时间为2h;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷;在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为400℃,保温时间为1h;所述极化的温度为80℃,极化电压为2kV/mm。
方案2:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料
各种原料根据化学式(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y和z均表示摩尔百分比,
其中x=0.6、y=0.2、z=0.02。
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3和BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;合成温度为800℃,保温时间为3h;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为4%;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;烧结温度为910℃,保温时间为3h;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷;在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为500℃,保温时间为2h;所述极化的温度为90℃,极化电压为3kV/mm。
方案3:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料
各种原料根据化学式(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y和z均表示摩尔百分比,
其中x=0.6、y=0.2、z=0.02。
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3和BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;合成温度为800℃,保温时间为3h;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为4%;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;烧结温度为910℃,保温时间为3h;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷;在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为500℃,保温时间为2h;所述极化的温度为90℃,极化电压为3kV/mm。
方案4:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料
各种原料根据化学式(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y和z均表示摩尔百分比,
其中x=0.6、y=0.23、z=0.02。
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3和BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;合成温度为900℃,保温时间为4h;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为5%;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;烧结温度为930℃,保温时间为4h;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷;在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为600℃,保温时间为3h;所述极化的温度为100℃,极化电压为4kV/mm。
方案5:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料
各种原料根据化学式(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y和z均表示摩尔百分比,
其中x=0.5、y=0.21、z=0.02。
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3和BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;合成温度为800℃,保温时间为3h;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为6%;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;烧结温度为940℃,保温时间为5h;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷;在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为650℃,保温时间为2.5h;所述极化的温度为120℃,极化电压为4.5kV/mm。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (9)
1.一种屏幕发声用压电陶瓷,包括以下列化学式I表示:(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7+zCuO,其特征在于:所述M选自Nb、Ta和Sb中的任意一种,所述x、y和z均表示摩尔百分比,所述z为CuO所占化合物(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7的摩尔百分比的数值,其中0.4<x<0.7,0.01<y<0.25,0<z<0.04,所述压电陶瓷处于三方和四方相共存状态。
2.根据权利要求1所述的一种屏幕发声用压电陶瓷,其特征在于:所述x、y和z,其中0.47≤x≤0.62,0.02≤y≤0.18,0.01≤z≤0.03。
3.根据权利要求1所述的一种屏幕发声用压电陶瓷,其特征在于:所述M为Nb。
4.根据权利要求1-3所述的任意一种屏幕发声用压电陶瓷的制备方法,具体包括如下步骤:
S1、配料:
以Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉末为原料,
各种原料根据化学式(1-y)(0.65Pb(Zr1-xTix)O3-0.35Pb(Ni0.33M0.67)O3)-yCa1.9Ba0.1Nb2O7设定值进行称量配料,
其中M选自Nb、Ta和Sb中的任意一种,
其中x、y均表示摩尔百分比,
其中0.4<x<0.7,0.01<y<0.25
S2、制备:
S21、合成:将Pb3O4、ZrO2、TiO2、NiO、M2O5、CaCO3以及BaCO3粉料混合物进行高温反应,以形成钙钛矿相结构的合成产物;
S22、造粒:将所述合成产物制备成粉末,并与CuO粉末进行混合,加入粘结剂进行造粒,以形成颗粒料;
S23、压制:将所述颗粒料装入模具中,压制成设定形状的粗坯;
S24、排胶:将粗坯进行排胶处理;
S25、烧结:将粗坯进行烧结,以获得致密的陶瓷元件;
S3、极化:
S31、将陶瓷元件进行极化,以得到压电陶瓷。
5.根据权利要求4所述的一种屏幕发声用压电陶瓷的制备方法,其特征在于:所述S21步骤中,合成温度为700-900℃,保温时间为2-4h。
6.根据权利要求4所述的一种屏幕发声用压电陶瓷及制备方法,其特征在于:所述S22步骤中,粘结剂为聚乙烯醇的水溶液,所述聚乙烯醇的水溶液的质量浓度为3%-10%。
7.根据权利要求4所述的一种屏幕发声用压电陶瓷及制备方法,其特征在于:所述S25步骤中,烧结温度为900-950℃,保温时间为2-6h。
8.根据权利要求4所述的一种屏幕发声用压电陶瓷及制备方法,其特征在于:所述S3步骤中,在进行极化之前,在所述陶瓷元件的两面被银,然后进行烧银,所述烧银的温度为400-700℃,保温时间为1-3h。
9.根据权利要求4所述的一种屏幕发声用压电陶瓷及制备方法,其特征在于:所述S3步骤中,所述极化的温度为80-140℃,极化电压为2-5kV/mm。
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