CN113603482A - 一种铌酸钾钠基无铅压电陶瓷及其制备方法 - Google Patents

一种铌酸钾钠基无铅压电陶瓷及其制备方法 Download PDF

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CN113603482A
CN113603482A CN202110767265.4A CN202110767265A CN113603482A CN 113603482 A CN113603482 A CN 113603482A CN 202110767265 A CN202110767265 A CN 202110767265A CN 113603482 A CN113603482 A CN 113603482A
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杜毅
刘伟朋
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Qilu University of Technology
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Abstract

本发明公开了一种铌酸钾基无铅压电陶瓷及其制备方法，所述铌酸钾钠基无铅压电陶瓷的化学计量比为：(1‑x)K0.48Na0.52NbO3‑x(NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3)，其中x=0，0.01，0.02，0.03，0.04，0.05，0.06。制备方法是将 K2CO3，Na2CO3，Li2CO3，Nb2O5，Sb2O5，Bi2O3，Sm2O3，ZrO2，这几种原料按照化学计量比称量好，进行配料，经过球磨、烘干后在870℃预烧6h得到预烧粉，再经过二次球磨、烘干、造粒、压片、排胶后，在1080‑1120℃下烧结，最后经过被银和极化操作后，制得较高压电常数的陶瓷片。本发明通过将 (NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3)掺杂在KNN基无铅压电陶瓷中，并对烧结工艺进行改进，提高了该压电陶瓷电学性能，其介电常数ε r =2000，居里温度T C =267℃，压电常数d 33 =340pC/N。

Description

一种铌酸钾钠基无铅压电陶瓷及其制备方法
技术领域
本发明涉及一种铌酸钾钠基无铅压电陶瓷及其制备方法，属于新型无铅基功能陶瓷领域。
背景技术
压电陶瓷是一种重要的功能陶瓷，可以用于实现将机械能与电能之间的相互转化，广泛应用于传感器，换能器，驱动器，变压器等领域。但是目前市场大规模使用的依旧是锆钛酸铅基（PZT）压电陶瓷。众所周知，含铅物具有毒性，在使用和处理过程中对人体和环境都会造成危害及污染。因此，研究和应用无铅的、环境友好且性能良好的压电陶瓷是很有价值和意义的。铌酸钾钠 (K，Na)NbO3基无铅压电陶瓷（简称KNN）因具有较高的居里温度和优异的介电、压电性能，受到人们的广泛关注，被认为是公认的最有可能取代铅基压电陶瓷的材料之一。然而，KNN陶瓷的制备工艺差，烧结温度较窄，碱金属元素K+、Na+在高温下极易挥发，采用传统制备工艺难以获得综合性能优良的无铅压电陶瓷。专利CN107857590 A采用的也是传统固相烧结技术，其特征在于掺杂Fe2+离子以提高KNN基压电陶瓷的电致应变以及逆压电系数，既可以降低陶瓷的烧结温度，又可以大幅提高基体陶瓷的应变性能，但是此方法得到的样品d 33 约为39~87pC/N。专利CN1810711A提出一种埋粉烧结方法，其特征是烧结时将陶瓷生坯埋在相同组分的粉体中，以防止K+、Na+的挥发，此法取得一定效果，但d 33 也仅有120 pC/N。专利CN1702055A采用织构化的方法制备无铅压电陶瓷，d 33 为123 pC/N，其制备工艺复杂，不适合大规模工业生产。
本发明的目的是在采用简单的制备工艺下制备出致密度高、综合性能良好的无铅压电陶瓷。与传统烧结方法相比，降低了生产成本、提升了电学性能，推进了无铅压电陶瓷的进一步发展。
发明内容
1.针对上述问题，本发明的目的是制备具有电学性能良好的铌酸钾钠基无铅压电陶瓷，旨在提供一种陶瓷生坯烧结方法，有效改善KNN基陶瓷的烧结性能和压电性能。
2.为实现上述技术目的，本发明技术方案为：
本发明的一种铌酸钾钠基无铅压电陶瓷及其制备方法，主要原料包括K2CO3，Na2CO3，Li2CO3，Nb2O5，Sb2O5，Bi2O3，Sm2O3，ZrO2其原料组分及其摩尔百分比含量为(1-x)K0.48Na0.52NbO3-x(NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3)，其中x=0，0.01，0.02，0.03，0.04，0.05，0.06。其特征在于所述制备方法包括以下步骤：
（1）配料，由(1-x)K0.48Na0.52NbO3-x(NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3) 的化学计量比称取原料K2CO3，Na2CO3，Li2CO3，Nb2O5，Sb2O5，Bi2O3，Sm2O3，ZrO2进行配料，将配好的原料放入氧化锆球为磨球的尼龙罐中，加入60ml无水乙醇进行球磨，获得混合均匀的浆料。将球磨后的浆料放置于60℃的烘箱中烘干12h；
（2）预烧，将烘干后的粉料进行研磨，再过80目筛，置于氧化铝坩埚中，在870℃马弗炉中预烧，保温3h，得到预烧粉料，将预烧后的粉料置于球磨机中进行二次球磨并烘干；
（3）造粒压片，将步骤（2）所得粉料过筛后，按照质量百分比7wt%加入聚乙烯醇(PVA)，充分研磨，再过筛得到颗粒均匀的粉料。将所得的粉料压制成直径为10mm，厚度为0.8-1.2mm的圆柱生坯；
（4）排胶，将步骤（3）所得生坯置于氧化铝坩埚中，并在550℃马弗炉中进行排胶，升温速率为1℃/min，保温时间为60min，随炉冷却到室温；
（5）烧结，将步骤（4）所得的陶瓷片，用同组分预烧粉进行埋粉后进行烧结，烧结制度为从室温以3℃/min的速率升温到1090℃并保温3h，然后随炉冷却，最终制得铌酸钾钠基无铅压电陶瓷样品；
（6）被银极化，对步骤（5）所制的陶瓷样品进行打磨抛光，并在两面均匀涂上银浆，然后将在550℃下保温60min烧成银电极。将被银后的陶瓷片置于硅油浴中进行极化，即得到(1-x)K0.48Na0.52NbO3-x(NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3)无铅压电陶瓷。
研究发现，烧结制度对KNN无铅压电陶瓷的烧结特性及电性能有很大影响，本发明用以上的技术方案，通过改进烧成制度曲线，可以制得致密度很高的陶瓷片。
本发明的有益效果：
（1）通过本发明的无铅压电陶瓷粉体的制备方法制得的KNN陶瓷片致密度均在致密度95%，相比传统固相烧结法致密度提高5%以上；
（2）通过本发明制备的KNN基无铅压电陶瓷具有良好的电性能，其介电常数ε r = 2000，，居里温度T C =267℃，d 33 =340pC/N。
附图说明
图1 (1-x)K0.48Na0.52NbO3-x(NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3)体系陶瓷样品的介电温谱图。

Claims (3)

1.这种铌酸钾钠基无铅压电陶瓷的制备方法，其特征在于组成原料及其摩尔百分比含量为(1-x)K0.48Na0.52NbO3-x(NaSbO3+(Bi0.45Sm0.05)Li0.5ZrO3)，其中x=0，0.01，0.02，0.03，0.04，0.05，0.06。
2.主要原料为：K2CO3，Na2CO3，Li2CO3，Nb2O5，Sb2O5，Bi2O3，Sm2O3，ZrO2。
3.权利要求1所述的一种铌酸钾钠基无铅压电陶瓷的制备方法，其特征在于，制备过程依次包括以下步骤：（1）将K2CO3，Na2CO3，Li2CO3，Nb2O5，Sb2O5，Bi2O3，Sm2O3，ZrO2粉末按照化学计量比进行配料、混合，将配好的原料放入以无水乙醇为介质、氧化锆球为磨球的尼龙罐中进行球磨，获得混合均匀的粉料，并在60℃烘箱中烘干12h；（2）将步骤（1）所得粉料过筛后进行预烧，预烧温度为870℃，时间为6h，升温速率为3℃/min，获得化学组分均匀的预烧粉，并进行二次球磨，将球磨后的浆料置于80℃烘箱中进行烘干12h；（3）将步骤（2）所得的粉料加入7wt%的聚乙烯醇(PVA)，进行充分的研磨后，过筛、压片、排胶，排胶温度为550℃，保温时间为60min，升温速率为1℃/min；（4）将步骤（3）所得的陶瓷片进行埋粉烧结，烧结时采取分段烧结，最佳烧结温度为1090℃，保温时间为3h，升温速率为2℃/min，由此获得高致密度的陶瓷片；（5）将步骤（4）所得的陶瓷片进行被银、极化，极化电场为3kV/mm，极化时间为30min，极化温度为60℃，最终获得铌酸钾钠基无铅压电陶瓷样品。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115321980A (zh) * 2022-07-13 2022-11-11 北京科技大学 一种铌酸钾钠(knn)基无铅压电陶瓷的制备方法
CN116477945A (zh) * 2022-12-05 2023-07-25 湖南大学 一种织构化的铌酸钾钠基压电陶瓷及其制备方法和应用

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115321980A (zh) * 2022-07-13 2022-11-11 北京科技大学 一种铌酸钾钠(knn)基无铅压电陶瓷的制备方法
CN116477945A (zh) * 2022-12-05 2023-07-25 湖南大学 一种织构化的铌酸钾钠基压电陶瓷及其制备方法和应用

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