CN108083798B - 无铅压电陶瓷组合物及其制备方法 - Google Patents

无铅压电陶瓷组合物及其制备方法 Download PDF

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CN108083798B
CN108083798B CN201711160342.XA CN201711160342A CN108083798B CN 108083798 B CN108083798 B CN 108083798B CN 201711160342 A CN201711160342 A CN 201711160342A CN 108083798 B CN108083798 B CN 108083798B
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苏蕊
李炳全
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Qianyue (Nanjing) integrated circuit industry Service Co.,Ltd.
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Abstract

本发明涉及用于压电元件的无铅压电陶瓷组合物，其包含：由(KaNabLic)eNbO3表示的铌酸盐作为第一相；a、b、c满足0.62<a≤0.68，0<b≤0.3，0<c≤0.2和a+b+c＝1；e满足1.01≤e≤1.09；和由SrLa(Mg1‑xSmx)O4表示的第二相；x满足3≤(1‑x)/x≤4.2；MnO2作为第一添加剂；Fe2O3作为第二添加剂；所述无铅压电陶瓷组合物，以摩尔百分比计，第二相含量为5‑11mol％，第一添加剂含量为0.5‑3mol％，第二添加剂含量为1‑4mol％，余量为第一相。

Description

无铅压电陶瓷组合物及其制备方法
技术领域
本发明涉及用于压电元件的无铅压电陶瓷组合物及其制备方法，特别是涉及一种无铅无铅压电陶瓷组合物及其制备方法。
背景技术
在压电陶瓷的领域里，一直占主导地位的是含铅的压电陶瓷，包括各种铅基压电复合钙钛矿铁电体。而在这些压电陶瓷中，铅的含量超过一半以上，这就难免在制作和使用过程中产生铅的污染，近年来在以欧洲为首的其他国家开始实施各种法令来限制铅在电子设备领域的使用时，意识到危机的中国也响应国际的号召对铅的使用做了不同程度的限制，这就需要开发新型的高性能的无铅压电陶瓷来满足日益增长的需求，这种需求也使得研究无铅压电陶瓷成为热门课题。
近年来，由于KNN体系无铅压电陶瓷具有其它体系压电陶瓷无法比拟的优势，毫无疑问地成了国内外科研工作者热捧的研究对象。KNN压电陶瓷通常用KNbO3、NaNbO3为初始原料，采用固相反应制备技术获得。近年来的很多研究显示，在KNN陶瓷制备时，通过加入其它化学成分进行改性，改性的KNN基压电陶瓷具有优良的电学性能，特别是还出现了良好的驰豫铁电性、光学性能。然而，直到现在，采用传统固相反应烧结工艺，依然很难制备高致密性的陶瓷体。
KNN压电陶瓷这种致命缺陷的存在被认为有以下两个重要因素:一个是在1140℃以上，KNN无法以固态形式存在，导致其只能在1140℃以才能以稳定的相存在，因而不能通过提高烧结温度来改善KNN陶瓷的烧结性能，増强陶瓷的致密性；二个是高温烧结时出现Na2O、K2O的挥发，这导致KNN的化学组分严重偏离其化学计量比,实验证实会产生K4Nb6O7的杂相物质，这种物质在环境潮湿时很容易潮解。这些缺陷很大程度上决定了KNN陶瓷在短期内很难有出色的表现。
纵览近年来的报道,世界各国科研人员采用很多有效的方法进行改善，以便获得良好的电学性能，常见的有:新组分引入，助熔剂添加，A、B位的取代，烧结工艺等措施，以便能解决这种缺陷，获得高性能、高致密性的压电陶瓷。
发明内容
为了解决现有技术中的上述技术问题，本发明的目的在于通过引入新组元，改善烧成技术，来改变当前烧结性差，以及电性能稳定性差的局面。
为了实现上述目的，本发明采用了以下技术方案：
一种无铅压电陶瓷组合物，其包含：由(KaNabLic)eNbO3表示的铌酸盐作为第一相；a、b、c满足0.62<a≤0.68，0<b≤0.3，0<c≤0.2和a+b+c＝1；e满足1.01≤e≤1.09；和由SrLa(Mg1-xSmx)O4表示的第二相；x满足3≤(1-x)/x≤4.2；MnO2作为第一添加剂；Fe2O3作为第二添加剂。
所述无铅压电陶瓷组合物，以摩尔百分比计，第二相含量为5-11mol％，第一添加剂含量为0.5-3mol％，第二添加剂含量为1-4mol％，余量为第一相。
所述无铅压电陶瓷组合物中，第一相中锰的含量大于第二相中锰的含量，第一相中锰的含量为所述无铅压电陶瓷组合物中锰含量的75％以上。
所述无铅压电陶瓷组合物的制备方法为：
根据第一相的组成称取K2CO3粉末、Na2CO3粉末、Li2CO3粉末和Nb2O5粉末，称取第一添加剂MnO2粉末；在原料粉末中加入乙醇，球磨机球磨5-8小时得到浆料；干燥浆料而得到混合粉末；在750℃～900℃下煅烧2-4小时合成第一相预煅烧粉末。
根据第二相的组成称取Sr2CO3粉末、La2O3粉末、MgO粉末和Sm2O3粉末；在原料粉末中加入乙醇，球磨机球磨5-8小时得到浆料；干燥浆料而得到混合粉末；在900℃～1050℃下煅烧4-6小时合成第二相预煅烧粉末。
按组成含量分别称量第一相预煅烧粉末、第二相预煅烧粉末和第二添加剂Fe2O3，加入分散剂、粘结剂以及乙醇球磨4-8小时形成浆料；对该浆料进行喷雾干燥、造粒，25-40MPa压力下压制成型；将所述成型体在600℃下保持2-4小时进行脱脂。
最后，将所述成型体在1050℃～1150℃的温度下烧结2～6小时，由此得到压电陶瓷。
本发明还涉及一种压电元件，其包括上述无铅压电陶瓷组合物形成的压电陶瓷体；和固定在所述压电陶瓷体的电极。
本发明的无铅压电陶瓷组合物及压电元件可以广泛用于振动检测、压力检测、振荡、以及压电器件等。例如可以用于：检测各种振动的传感器类、致动器、高电压产生装置、各种驱动装置、位置控制装置、振动抑制装置、流体喷出装置等各种装置。
具体实施方式
以下将结合具体实施例对本发明所述的无铅压电陶瓷组合物做进一步的阐述，以对本发明的发明构思及其效果做出更完整的说明。
根据第一相的组成称取K2CO3粉末、Na2CO3粉末、Li2CO3粉末和Nb2O5粉末，称取第一添加剂MnO2粉末；在原料粉末中加入乙醇，球磨机球磨6小时得到浆料；干燥浆料而得到混合粉末；在850℃下煅烧3小时合成第一相预煅烧粉末。
根据第二相的组成称取Sr2CO3粉末、La2O3粉末、MgO粉末和Sm2O3粉末；在原料粉末中加入乙醇，球磨机球磨6小时得到浆料；干燥浆料而得到混合粉末；在1050℃下煅烧5小时合成第二相预煅烧粉末。
按组成含量分别称量第一相预煅烧粉末、第二相预煅烧粉末和第二添加剂Fe2O3，加入分散剂、粘结剂以及乙醇球磨8小时形成浆料；对该浆料进行喷雾干燥、造粒，25MPa压力下压制成型；将所述成型体在600℃下保持3小时进行脱脂。
最后，将所述成型体在1050℃的温度下烧结5小时，由此得到压电陶瓷。
依据压电元件所要求的尺寸精度对压电陶瓷进行加工；在由此得到的压电陶瓷上镀银电极，进行极化处理。测定压电元件的相对介电常数ε33 T/ε0、压电常数d33、机电耦合系数kr。
测试结果见表1
表1
Figure BDA0001474798710000031
Figure BDA0001474798710000041
对于本领域的普通技术人员而言，具体实施例只是对本发明进行了示例性描述，本发明具体实现并不受上述方式的限制，只要采用了本发明的方法构思和技术方案进行的各种非实质性的改进，或未经改进将本发明的构思和技术方案直接应用于其它场合的，均在本发明的保护范围之内。

Claims (3)

1.一种无铅压电陶瓷组合物，其特征在于：其包含：由(KaNabLic)eNbO3表示的铌酸盐作为第一相；a、b、c满足0.62<a≤0.68，0<b≤0.3，0<c≤0.2和a+b+c＝1；e满足1.01≤e≤1.09；和由SrLa(Mg1-xSmx)O4表示的第二相；x满足3≤(1-x)/x≤4.2；MnO2作为第一添加剂；Fe2O3作为第二添加剂；所述无铅压电陶瓷组合物，以摩尔百分比计，第二相含量为5-11mol％，第一添加剂含量为0.5-3mol％，第二添加剂含量为1-4mol％，余量为第一相；所述无铅压电陶瓷组合物中，第一相中锰的含量为所述无铅压电陶瓷组合物中锰含量的75％以上。
2.一种如权利要求1所述无铅压电陶瓷组合物的制备方法，其特征在于：包括以下步骤：根据第一相的组成称取K2CO3粉末、Na2CO3粉末、Li2CO3粉末和Nb2O5粉末，称取第一添加剂MnO2粉末；在原料粉末中加入乙醇，球磨机球磨5-8小时得到浆料；干燥浆料而得到混合粉末；在750℃～900℃下煅烧2-4小时合成第一相预煅烧粉末；根据第二相的组成称取Sr2CO3粉末、La2O3粉末、MgO粉末和Sm2O3粉末；在原料粉末中加入乙醇，球磨机球磨5-8小时得到浆料；干燥浆料而得到混合粉末；在900℃～1050℃下煅烧4-6小时合成第二相预煅烧粉末；按组成含量分别称量第一相预煅烧粉末、第二相预煅烧粉末和第二添加剂Fe2O3，加入分散剂、粘结剂以及乙醇球磨4-8小时形成浆料；对该浆料进行喷雾干燥、造粒，25-40MPa压力下压制成型；将所述成型体在600℃下保持2-4小时进行脱脂；最后，将所述成型体在1050℃～1150℃的温度下烧结2～6小时，由此得到无铅压电陶瓷组合物。
3.一种压电元件，其特征在于：其包括：由根据权利要求1所述的无铅压电陶瓷组合物形成的压电陶瓷体；和固定在所述压电陶瓷体的电极。
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