CN108623302A - 一种无铅压电纳米阵列及其制备方法 - Google Patents

一种无铅压电纳米阵列及其制备方法 Download PDF

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CN108623302A
CN108623302A CN201810670156.9A CN201810670156A CN108623302A CN 108623302 A CN108623302 A CN 108623302A CN 201810670156 A CN201810670156 A CN 201810670156A CN 108623302 A CN108623302 A CN 108623302A
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周昌荣
许积文
曾卫东
黎清宁
杨玲
袁昌来
陈国华
饶光辉
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Abstract

本发明公开了一种无铅压电纳米阵列及其制备方法，材料组成为：0.9Bi0.5Na0.5TiO3‑0.1Bi2(Mn4/3Ni2/3)O3。通过Bi0.5Na0.5TiO3和A位纯Bi的Bi2(Mn4/3Ni2/3)O3铁电体复合，结合固相烧结及热处理技术，生长纳米阵列，其中纳米线长度在2‑10μm，直径为60‑800nm，工艺简单，产率高，成本低廉，适合大规模工业生产。

Description

一种无铅压电纳米阵列及其制备方法
技术领域
本发明涉及的无铅铁电材料，具体是一种ABO3型钙钛矿结构，无铅压电纳米阵列及其制备方法。
背景技术
—维压电纳米结构主要包括纳米管，纳米纤维，纳米线以及量子点等。与薄膜不同，纳米线、纳米管等一维材料有更高的比表面积，更高的长径比，具有比薄膜和纳米颗粒更优异的性质，可以大幅缩小器件体积、提高性能，便于集成化制造。而且这些结构不仅具有一些特殊特点如晶体学取向，混合相组成，电畴结构，以及有限尺寸的极化响应等，而且还具有某些特殊的效应例如表界面效应，隧道效应，半导体性铁电体的电子运输等很可能使得铁电一维纳米材料在性能上发生质的变化。一维纳米材料的合成方法有很多种，早期的有纳米平板印刷术如电子束离子束刻蚀、射线或远紫外光刻等，目前兴起的还有化学法。通过纳米平板印刷术制备一维纳米材料的目标性强，而且可以较好的控制材料的微观尺寸，但是这一类方法存在着普遍的缺陷，即生产成本过高且不易实现工业生产。
常见的纳米阵列化学合成方法有模板法、金属溶盐法、水热法和溶胶凝胶法等。但是这些制备方法对材料的种类、生产成本、材料产量和产率方面的都存在不足。通过固相烧结结合热处理制备无铅压电纳米阵列还未见报导。
发明内容
本发明的目的是提供一种ABO3型钙钛矿结构，无铅压电纳米阵列及制备方法，通过Bi0.5Na0.5TiO3和A位纯Bi的Bi2(Mn4/3Ni2/3)O3铁电体复合，以及固相烧结法与热处理三者有机结合，生长长度在3-8μm，直径为100-500nm的纳米阵列，具有产率高、工艺简单、成本低、易于实现、适合大规模工业生产的优点。
本发明一种无铅压电纳米阵列，材料组成为：
0.9Bi0.5Na0.5TiO3-0.1Bi2(Mn4/3Ni2/3)O3。
本发明无铅压电纳米阵列的制备方法，采用传统陶瓷烧结法，结合热处理技术，具体包括如下步骤：
(1)按照Bi0.5Na0.5TiO3的化学计量分别称取分析纯原料Bi2O3、Na2CO3和TiO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干，再在高铝坩埚中于850℃保温2小时预合成Bi0.5Na0.5TiO3粉体；
(2)按照Bi2(Mn4/3Ni2/3)O3的化学计量分别称取分析纯原料Bi2O3、NiO和MnO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干，再在高铝坩埚中于760℃保温2小时预合成Bi2(Mn4/3Ni2/3)O3粉体；
(3)将合成好的Bi0.5Na0.5TiO3、Bi2(Mn4/3Ni2/3)O3粉体，按照0.9Bi0.5Na0.5TiO3-0.1Bi2(Mn4/3Ni2/3)O3化学计量式配料，以无水乙醇为介质球磨15h，干燥，加入5%的PVA造粒；在100Mpa压力下冷等静压成型；
(4)成型的原料采用微波烧结，990℃保温20分钟，烧结成瓷；
(5)烧结的样品放在氧化锆板上，上面覆盖氧化铝板，58℃/min快速升温至635℃保温95分钟，然后随炉冷却至室温，通过热处理的样品生长成无铅压电纳米阵列，其中纳米线长度在2-10μm，直径为60-800nm。
采用本发明方法制备的无铅压电纳米阵列，长度在2-10μm，直径为60-800nm，具有产率高、工艺简单、成本低、易于实现、适合大规模工业生产的优点。
附图说明
图1为本发明无铅压电纳米阵列的SEM图。
具体实施方式
下面结合实施例和附图对本发明内容作进一步的说明，但不是以本发明的限定。
实施例
本发明无铅压电纳米阵列材料，组成为：
0.9Bi0.5Na0.5TiO3-0.1Bi2(Mn4/3Ni2/3)O3；制备方法包括如下步骤：
(1)按照Bi0.5Na0.5TiO3的化学计量分别称取分析纯原料Bi2O3、Na2CO3和TiO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干, 再在高铝坩埚中于850℃保温2小时预合成Bi0.5Na0.5TiO3粉体；
(2)按照Bi2(Mn4/3Ni2/3)O3的化学计量分别称取分析纯原料Bi2O3、NiO和MnO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干, 再在高铝坩埚中于760℃保温2小时预合成Bi2(Mn4/3Ni2/3)O3粉体；
(3)将合成好的Bi0.5Na0.5TiO3、Bi2(Mn4/3Ni2/3)O3粉体，按照0.9Bi0.5Na0.5TiO3-0.1Bi2(Mn4/3Ni2/3)O3化学计量式配料，以无水乙醇为介质球磨15h，干燥，加入5%的PVA造粒；在100Mpa压力下冷等静压成型；
(4)成型的原料采用微波烧结，990℃保温20分钟，烧结成瓷；
(5)烧结的样品放在氧化锆板上，上面覆盖氧化铝板，58℃/min快速升温至635℃保温95分钟，然后随炉冷却至室温；通过热处理的样品生长成压电纳米阵列，其SEM图，如图1所示，其中纳米线长度在2-10μm，直径为60-800nm。
通过上面给出的实施例，可以进一步清楚的了解本发明的内容，但它们不是对本发明的限定。

Claims (2)

1.一种无铅压电纳米阵列，其特征在于：该无铅压电纳米阵列的组成为：0.9Bi0.5Na0.5TiO3-0.1Bi2(Mn4/3Ni2/3)O3。
2.根据权利要求1所述的无铅压电纳米阵列的制备方法，其特征在于，包括如下步骤：
（1）按照Bi0.5Na0.5TiO3的化学计量分别称取分析纯原料Bi2O3、Na2CO3和TiO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干, 再在高铝坩埚中于850℃保温2小时预合成Bi0.5Na0.5TiO3粉体；
（2）按照Bi2(Mn4/3Ni2/3)O3的化学计量分别称取分析纯原料Bi2O3、NiO和MnO2，装入球磨罐中，以氧化锆为磨球、无水乙醇为球磨介质，充分混合球磨24小时，分离磨球，将原料在60℃烘干, 再在高铝坩埚中于760℃保温2小时预合成Bi2(Mn4/3Ni2/3)O3粉体；
（3）将合成好的Bi0.5Na0.5TiO3、Bi2(Mn4/3Ni2/3)O3粉体，按照0.9Bi0.5Na0.5TiO3-0.1Bi2(Mn4/3Ni2/3)O3化学计量式配料，以无水乙醇为介质球磨15h，干燥，加入5%的PVA造粒；在100Mpa压力下冷等静压成型；
（4）成型的原料采用微波烧结，990℃保温20分钟，烧结成瓷；
（5）烧结的样品放在氧化锆板上，上面覆盖氧化铝板，58℃/min快速升温至635℃保温95分钟，然后随炉冷却至室温；通过热处理的样品生长成无铅压电纳米阵列，其中纳米线长度在2-10μm，直径为60-800nm。
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