CN110550953A - 一种钛酸铋钠基无铅压电陶瓷及其制备方法 - Google Patents

一种钛酸铋钠基无铅压电陶瓷及其制备方法 Download PDF

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CN110550953A
CN110550953A CN201910873427.5A CN201910873427A CN110550953A CN 110550953 A CN110550953 A CN 110550953A CN 201910873427 A CN201910873427 A CN 201910873427A CN 110550953 A CN110550953 A CN 110550953A
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free piezoelectric
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杜毅
王佳佳
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Qilu University of Technology
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Abstract

本发明公开了一种钛酸铋钠基无铅压电陶瓷及其制备方法，所述钛酸铋钠基无铅压电陶瓷的化学计量比为：（1‑x)Bi0.5(Na0.48K0.52)0.5TiO3‑xBaZrO3，其中x=0，0.03，0.06，0.09。制备方法包括：将Bi2O3，K2CO3，Na2CO3，TiO2，ZrO2粉末按照化学计量比进行配料，经过球磨、烘干后，在850℃预烧2.5h得到预烧粉，再经过二次球磨、烘干、造粒、压片、排胶后，于1100℃烧结，最后经过被银和极化，制得高致密度的陶瓷片。本发明通过将锆元素掺杂在钛酸铋钠基无铅压电陶瓷中，并对烧结工艺进行改进，提高了压电陶瓷的致密度及介电性能，使得所制钛酸铋钠基无铅压电陶瓷的介电常数最高可达εr=2945，TC=372℃。致密度较传统烧结工艺提升8%左右。

Description

一种钛酸铋钠基无铅压电陶瓷及其制备方法
技术领域
本发明涉及一种钛酸铋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。
无铅压电材料中，钛酸铋钠（Bi0.5Na0.5TiO3，简称BNT）因其具有较高的剩余极化强度以及居里温度，被认为是最有希望取代铅基压电陶瓷的无铅体系之一。但总体来说，钛酸铋钠基无铅压电陶瓷的介电性能方面仍需进行改进。专利CN109574656A提出一种高储能钛酸铋钠-钛酸锶钡基介质材料及其制备方法，但是所用的原料种类较多，价格昂贵，实验过程相对复杂，不适合大规模的工业化生产。专利CN108147813A提出一种高压电系数钛酸铋钠基无铅压电陶瓷及其制备方法，其特征在于通过Rb等价掺杂的方法，使其具有比纯BNT陶瓷更加优异的烧结特性和压电性能，但所得材料的介电性能较差，使得应用方面不够广泛。
为了进一步提高钛酸铋钠基无铅压电陶瓷的介电性能，通常采用添加第二组元的方法进行掺杂改性。本发明采用了对BNT体系进行Zr4+等价掺杂的方法，对其介电性能进行改进，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高介电系数的钛酸铋钠基无铅压电陶瓷，旨在提供一种陶瓷生坯烧结方法，有效改善BNT陶瓷的烧结性能和介电性能。
2.为实现上述技术目的，本发明技术方案为：
本发明的一种钛酸铋钠基无铅压电陶瓷及其制备方法，主要原料包括Bi2O3，K2CO3，Na2CO3，TiO2，ZrO2，其原料组分及其摩尔百分比含量为（1-x)Bi0.5(Na0.48K0.52)0.5TiO3-xBaZrO3，其中x=0，0.03，0.06，0.09。其特征在于，所述制备方法包括以下步骤：
（1）配料
根据(1-x)Bi0.5(Na0.48K0.52)0.5TiO3-xBaZrO3的化学计量比称取原料Bi2O3，K2CO3，Na2CO3，TiO2，ZrO2。进行配料，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。将球磨后的浆料于60℃的烘箱中烘干24h；
（2）预烧
将烘干后的粉料进行研磨并过筛后置于氧化铝坩埚中，在850℃马弗炉中预烧2.5h，得到预烧粉料，将所得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5wt%加入聚乙烯醇（PVA），充分研磨在，得到颗粒均匀的粉料。将所得的粉料压制成直径为12mm，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2℃/min，保温时间为30min，其后随炉自然冷却；
（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，烧结制度为首先从室温以3℃/min的速率升温到850℃，保温2.5h,再以2℃/min升温到1100℃并保温3h，其后随炉自然冷却，最终制得钛酸铋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，并在两面均匀涂上中温银浆，在550℃下保温30min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)Bi0.5(Na0.48K0.52)0.5TiO3-xBaZrO3无铅压电陶瓷。
3.根据权利要求2所述的一种高介电系数钛酸铋钠基无铅压电陶瓷的制备方法，其特征在于步骤（1）中所述的料：球：水（乙醇）比为1:2:1.5。
4.根据权利要求2所述的一种高介电系数钛酸铋钠基无铅压电陶瓷的制备方法，其特征在于步骤（1）和（2）中的球磨机的转速均为300r/min,球磨时间均为15h。
5. 根据权利要求2所述的一种高介电系数钛酸铋钠基无铅压电陶瓷的制备方法，其特征在于步骤（2）中的预烧时间为2.5h。
6. 根据权利要求2所述的一种高介电系数钛酸铋钠基无铅压电陶瓷的制备方法，其特征在于步骤（4）中压制生坯时的压强为25Mpa，保压时间为1min。
7. 根据权利要求2所述的一种高介电系数钛酸铋钠基无铅压电陶瓷的制备方法，其特征在于步骤（6）中的极化时间为30min，极化电场为4-6kV/mm。
研究发现，烧结制度对BNT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BNT陶瓷片致密度均在92%以上，相比传统固相烧结法致密度提高8%以上。（2）通过本发明制备的BNT基无铅压电陶瓷具有良好的电性能，其介电常数εr=2945，介电损耗tanδ=6.2%，TC=372℃，机电耦合系数kp=27.2%。
附图说明
下面结合附图和具体实施方式对本发明做进一步阐述：
图1是(1-x)Bi0.5(Na0.48K0.52)0.5TiO3-xBaZrO3体系陶瓷样品的XRD图。
图2是(1-x)Bi0.5(Na0.48K0.52)0.5TiO3-xBaZrO3体系陶瓷样品的介电温谱图。

Claims (2)

1.一种钛酸铋钠基无铅压电陶瓷及其制备方法，其特征在于，组成原料及其摩尔百分比含量为（1-x)Bi0.5(Na0.48K0.52)0.5TiO3-xBaZrO3，其中x=0，0.03，0.06，0.09，主要原料包括Bi2O3，K2CO3，Na2CO3，TiO2，ZrO2。
2.权利要求1所述的一种钛酸铋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Bi2O3，K2CO3，Na2CO3，TiO2，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24h；
（2）将步骤（1）所得粉料过筛后进行预烧，预烧温度为850℃，时间为2.5h，升温速率为3℃/min，获得化学组分均一的预烧粉，并进行二次球磨，置于80℃烘箱中进行烘干24h；
（3）将步骤（2）所得的粉料加入5wt %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30min，升温速率为2℃/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，最高烧结温度为1100℃，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5kV/mm，极化时间为30min，极化温度为80℃，最终获得钛酸铋钠基无铅压电陶瓷样品。
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN111041548A (zh) * 2019-11-21 2020-04-21 广东工业大学 一种板状钛酸铋钠模板晶粒及其制备方法和应用
CN116444264A (zh) * 2023-04-18 2023-07-18 北京科技大学 一种具有优异储能性能及环境稳定性的钛酸铋钾钠基弛豫铁电陶瓷材料及其制备方法
CN116606138A (zh) * 2022-02-08 2023-08-18 成都理想境界科技有限公司 一种压电陶瓷及其制备方法和应用

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111041548A (zh) * 2019-11-21 2020-04-21 广东工业大学 一种板状钛酸铋钠模板晶粒及其制备方法和应用
CN111041548B (zh) * 2019-11-21 2021-12-17 广东工业大学 一种板状钛酸铋钠模板晶粒及其制备方法和应用
CN116606138A (zh) * 2022-02-08 2023-08-18 成都理想境界科技有限公司 一种压电陶瓷及其制备方法和应用
CN116444264A (zh) * 2023-04-18 2023-07-18 北京科技大学 一种具有优异储能性能及环境稳定性的钛酸铋钾钠基弛豫铁电陶瓷材料及其制备方法
CN116444264B (zh) * 2023-04-18 2024-05-17 北京科技大学 一种具有优异储能性能及环境稳定性的钛酸铋钾钠基弛豫铁电陶瓷材料及其制备方法

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