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CN113773078A - 一种大功率型压电陶瓷材料及其制备方法 - Google Patents

一种大功率型压电陶瓷材料及其制备方法 Download PDF

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CN113773078A
CN113773078A CN202111249010.5A CN202111249010A CN113773078A CN 113773078 A CN113773078 A CN 113773078A CN 202111249010 A CN202111249010 A CN 202111249010A CN 113773078 A CN113773078 A CN 113773078A
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余健
蒋杏兵
张晖
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Haiying Enterprise Group Co Ltd
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Abstract

本发明涉及一种大功率型压电陶瓷材料及其制备方法，其主要成分为锆钛酸铅固溶体，可不掺杂或可掺杂选自Fe2O3、Ta2O3、CaCO3、BaCO3和SiO2中的至少2种和几种添加物。包括如下步骤：配料：陶瓷配方为PbxSr1‑x(ZryTi1‑y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2，混料，预烧，二次球磨，增塑，成型与排塑，烧结，上电极和极化处理，压电性能测量。本发明的压电陶瓷材料在PZT系列压电陶瓷的基础上，引入Fe2O3、Ta2O3、CaCO3、BaCO3和SiO2等物质有助于改善陶瓷的各项压电性能，同时使用本发明申请的制备方法得到的陶瓷材料具有低损耗和高介电性，适用于大功率型水声材料。

Description

一种大功率型压电陶瓷材料及其制备方法
技术领域
本发明涉及压电陶瓷材料技术，尤其是指一种大功率型压电陶瓷材料及其制备方法。
背景技术
PZT压电陶瓷材料是一种应用极为广泛的功能材料，通过压电效应可实现电能和机械能的相互转化。PZT基压电陶瓷具有机电耦合系数高、容易加工成复杂形状、价格低廉、易于批量生产等优点，已被广泛应用于电子器件中。但是，现有的压电陶瓷材料尚不能满足实际应用对材料性能的综合要求。随着现代工业的快速发展，对高性能和低损耗的压电陶瓷提出了更高的要求。
目前为改进压电陶瓷的工作性能，常根据不同掺杂离子对材料结构和性能的影响不同，对现有压电陶瓷进行掺杂改性PZT系列压电陶瓷。由于掺杂的作用机制非常复杂，探索微观结构和电性能之间的内在规律一直是近年来研究人员的研究重点。
发明内容
为此，本发明所要解决的技术问题在于克服现有压电陶瓷材料尚不能满足实际应用对材料性能的综合要求的问题，从而提供一种大功率型压电陶瓷材料及其制备方法。
为解决上述技术问题，本发明的一种大功率型压电陶瓷材料及其制备方法，其主要成分为锆钛酸铅固溶体，可不掺杂或可掺杂选自Fe2O3、Ta2O3、CaCO3、BaCO3和SiO2中的至少2种和几种添加物。包括如下步骤：
步骤S1，配料：陶瓷配方为PbxSr1-x(ZryTi1-y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2；其中x、y为摩尔比，a、b、c、d、e为重量比，0.91≤x≤0.97，0.51≤y≤0.55，0.15％≤a≤0.25％，0.2％≤b≤0.3％，0.5％≤c≤0.45％，0.15％≤d≤0.2％，0.1％≤e≤0.15％，根据化学分子式计算各组分比例并配制；
步骤S2，混料：采用传统湿法球磨混料，将陶瓷粉料和去离子水按照100:45的质量比加入搅拌桶；
步骤S3，预烧：生成压电陶瓷的过程是一种典型的化学反应过程，在比熔点低的温度下，Pb原子可以通过扩散到其他材料晶体中，生成PbZrTiO3；
步骤S4，二次球磨：称取预烧处理后的陶瓷粉末倒入去离子水中并搅拌均匀，制成混合陶瓷料浆；
步骤S5，增塑：将细化后的陶瓷料浆从料筒中取出；把陶瓷料浆与占料重5％左右的PVA溶液球磨搅拌混合均匀，将陶瓷料浆接入喷雾造粒机，制备得到的粉体用100目筛网进一步过筛；
步骤S6，成型与排塑：将粉末预压成型，排塑：将陶瓷素坯放入马弗炉，设置最高温度750℃，进一步排除陶瓷素坯中的成型剂；
步骤S7，烧结：实验设置烧结温度为1290-1330℃，保温2h，随炉冷却；
步骤S8，上电极和极化处理，上电极：在压电陶瓷表面进行渗银处理，形成金属薄膜，极化处理：对压电陶瓷施加一个强直流电场；
步骤S9，压电性能测量：如d33、介质损耗tanδ、机电耦合系数Kp。
在本发明的一个实施例中，所述的混料步骤中采用料浆需要预先在搅拌桶中搅拌5min，低速球磨30s后，无异常开始高速球磨，球磨的时间设置为4h，球磨结束，将料浆烘干备用。
在本发明的一个实施例中，所述的二次球磨步骤中将混合陶瓷料浆填入球磨机的料筒中进行二次细化处理24h。
所述的成型与排塑步骤中将圆晶片设置预压成型尺寸为20x1mm。
在本发明的一个实施例中，所述的压电陶瓷经过极化处理步骤后，其材料内部的铁电畴发生转向，陶瓷中的电畴全部按电场方向排列，只有经过极化处理的压电陶瓷材料才有压电效应。
本发明的上述技术方案相比现有技术具有以下优点：本发明的压电陶瓷材料在PZT系列压电陶瓷的基础上，引入Fe2O3、Ta2O3、CaCO3、BaCO3和SiO2等物质有助于改善陶瓷的各项压电性能，同时使用本发明申请的制备方法得到的陶瓷材料具有低损耗和高介电性，适用于大功率型水声材料。
附图说明
为了使本发明的内容更容易被清楚的理解，下面根据本发明的具体实施例并结合附图，对本发明作进一步详细的说明。
图1是一种大功率型压电陶瓷材料及其制备方法流程图。
具体实施方式
如图1所示，本实施例提供一种大功率型压电陶瓷材料及其制备方法，其主要成分为锆钛酸铅固溶体，可不掺杂或可掺杂选自Fe2O3、Ta2O3、CaCO3、BaCO3和SiO2中的至少2种和几种添加物。包括如下步骤：
步骤S1，配料：陶瓷配方为PbxSr1-x(ZryTi1-y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2；其中x、y为摩尔比，a、b、c、d、e为重量比，0.91≤x≤0.97，0.51≤y≤0.55，0.15％≤a≤0.25％，0.2％≤b≤0.3％，0.5％≤c≤0.45％，0.15％≤d≤0.2％，0.1％≤e≤0.15％，根据化学分子式计算各组分比例并配制；
步骤S2，混料：采用传统湿法球磨混料，将陶瓷粉料和去离子水按照100:45的质量比加入搅拌桶；
步骤S3，预烧：生成压电陶瓷的过程是一种典型的化学反应过程，在比熔点低的温度下，Pb原子可以通过扩散到其他材料晶体中，生成PbZrTiO3；
步骤S4，二次球磨：称取预烧处理后的陶瓷粉末倒入去离子水中并搅拌均匀，制成混合陶瓷料浆；
步骤S5，增塑：将细化后的陶瓷料浆从料筒中取出；把陶瓷料浆与占料重5％左右的PVA溶液球磨搅拌混合均匀，将陶瓷料浆接入喷雾造粒机，制备得到的粉体用100目筛网进一步过筛；
步骤S6，成型与排塑：将粉末预压成型，排塑：将陶瓷素坯放入马弗炉，设置最高温度750℃，进一步排除陶瓷素坯中的成型剂，保证烧结质量，提高烧结致密度；
步骤S7，烧结：实验设置烧结温度为1300℃，保温2h，随炉冷却；
步骤S8，上电极和极化处理，上电极：在压电陶瓷表面进行渗银处理，形成金属薄膜，极化处理：对压电陶瓷施加一个强直流电场；
步骤S9，压电性能测量：如d33、介质损耗tanδ、机电耦合系数Kp。
其中20x1mm圆晶片实验测量结果如下：
Figure BDA0003321822380000031
水声材料大功率型压电材料(P-8)一般性能参数：
Figure BDA0003321822380000032
结论：
该方法制备的大功率型陶瓷材料介质损耗为tanδ(％)＝0.25，在常温下d33值为285pC/N，常温下kp＝59％，达到了水声材料应用的性能标准。此外，该方法制备的材料相对一般大功率压电材料具有较高的介电常数，具有更多的应用场合。
所述的混料步骤中采用料浆需要预先在搅拌桶中搅拌5min，低速球磨30s后，无异常开始高速球磨，球磨的时间设置为4h，球磨结束，将料浆烘干备用。
所述的二次球磨步骤中将混合陶瓷料浆填入球磨机的料筒中进行二次细化处理24h。
所述的成型与排塑步骤中将圆晶片设置预压成型尺寸为20x1mm。
所述的压电陶瓷经过极化处理步骤后，其材料内部的铁电畴发生转向，陶瓷中的电畴全部按电场方向排列，只有经过极化处理的压电陶瓷材料才有压电效应。
显然，上述实施例仅仅是为清楚地说明所作的举例，并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (5)

1.一种大功率型压电陶瓷材料及其制备方法，其特征在于，包括如下步骤：
步骤S1，配料：陶瓷配方为PbxSr1-x(ZryTi1-y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2；其中x、y为摩尔比，a、b、c、d、e为重量比，0.91≤x≤0.97，0.51≤y≤0.55，0.15％≤a≤0.25％，0.2％≤b≤0.3％，0.5％≤c≤0.45％，0.15％≤d≤0.2％，0.1％≤e≤0.15％，根据化学分子式计算各组分比例并配制；
步骤S2，混料：采用传统湿法球磨混料，将陶瓷粉料和去离子水按照100:45的质量比加入搅拌桶；
步骤S3，预烧：生成压电陶瓷的过程是一种典型的化学反应过程，在比熔点低的温度下，Pb原子可以通过扩散到其他材料晶体中，生成PbZrTiO3；
步骤S4，二次球磨：称取预烧处理后的陶瓷粉末倒入去离子水中并搅拌均匀，制成混合陶瓷料浆；
步骤S5，增塑：将细化后的陶瓷料浆从料筒中取出；把陶瓷料浆与占料重5％左右的PVA溶液球磨搅拌混合均匀，将陶瓷料浆接入喷雾造粒机，制备得到的粉体用100目筛网进一步过筛；
步骤S6，成型与排塑：将粉末预压成型，排塑：将陶瓷素坯放入马弗炉，设置最高温度750℃，进一步排除陶瓷素坯中的成型剂；
步骤S7，烧结：实验设置烧结温度为1290-1330℃，保温2h，随炉冷却；
步骤S8，上电极和极化处理，上电极：在压电陶瓷表面进行渗银处理，形成金属薄膜，极化处理：对压电陶瓷施加一个强直流电场；
步骤S9，压电性能测量：如d33、介质损耗tanδ、机电耦合系数Kp。
2.根据权利要求1所述的一种大功率型压电陶瓷材料及其制备方法，其特征在于：所述的混料步骤中采用料浆需要预先在搅拌桶中搅拌5min，低速球磨30s后，无异常开始高速球磨，球磨的时间设置为4h，球磨结束，将料浆烘干备用。
3.根据权利要求1所述的一种大功率型压电陶瓷材料及其制备方法，其特征在于：所述的二次球磨步骤中将混合陶瓷料浆填入球磨机的料筒中进行二次细化处理24h。
4.根据权利要求1所述的一种大功率型压电陶瓷材料及其制备方法，其特征在于：所述的成型与排塑步骤中将圆晶片设置预压成型尺寸为20x1mm。
5.根据权利要求1所述的一种大功率型压电陶瓷材料及其制备方法，其特征在于：所述的压电陶瓷经过极化处理步骤后，其材料内部的铁电畴发生转向，陶瓷中的电畴全部按电场方向排列，只有经过极化处理的压电陶瓷材料才有压电效应。
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Application publication date: 20211210