CN113999006B - 具有晶界颗粒桥结构的高温细晶能量收集压电陶瓷材料及制备 - Google Patents
具有晶界颗粒桥结构的高温细晶能量收集压电陶瓷材料及制备 Download PDFInfo
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Abstract
具有晶界颗粒桥结构的高温细晶能量收集压电陶瓷材料及制备，属于高温压电材料技术领域。陶瓷晶界处存在规律性排布的纳米级颗粒，且晶界纳米颗粒与陶瓷晶粒内部具有协同的铁电畴。这种特殊晶界颗粒桥结构的存在，使得高温压电陶瓷可以同时获得小晶粒尺寸和高压电性能，进而获得高的换能系数，在高温细晶压电能量收集器应用领域具有十分重要的应用前景。
Description
技术领域
本发明属于高温压电材料技术领域，具体涉及一种可实现高温细晶压电陶瓷同时具有小晶粒尺寸和高压电性能的结构设计策略及制备方法。
背景技术
在能源日益紧缺的当下，如何将环境中废弃的振动能转化为电能应用于电子设备供电变得尤其重要。基于压电材料独特的正压电效应，可实现清洁发电的压电能量收集器受到全球性的关注。近年来，在航空航天、新能源汽车和石油勘探等领域，自供电无线微型传感器需要在极端高温环境下稳定工作，因此可驱动无线微型传感器的高温能量收集用压电陶瓷不仅要具有远小于1μm的细晶级晶粒尺寸以保证力学可靠性和便于低尺度集成，同时也要保持高换能系数以获得高发电特性。然而，从以往的研究发现，压电陶瓷的晶粒尺寸与压电性能之间存在协同效应，难以在小晶粒尺寸时获得良好的换能系数。
究其原因是普通压电陶瓷主要由结晶晶粒和非晶相晶界所构成。晶粒越小，非晶相晶界的含量越高，在外加电场下，其对陶瓷晶粒内部电畴翻转的阻碍作用越严重，从而导致陶瓷压电性能降低。若要在保持小晶粒尺寸的同时提升细晶压电陶瓷的压电性能，则必须改变普通细晶压电陶瓷的非晶相晶界结构。
在本发明中，我们首次提出替代非晶相晶界结构的晶界颗粒桥结构这一新型高性能细晶压电陶瓷设计策略，即将普通细晶陶瓷的非晶相晶界替换为含有连续的纳米颗粒构成的桥接型晶界(晶界颗粒桥结构)。以0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3(缩写为BS-PT-PIN)为研究体系，成功制备出晶界颗粒桥结构的致密高温细晶压电陶瓷，在具有小晶粒尺寸的同时具有高换能系数，打破晶粒尺寸与压电性能间的耦合关系。该策略的提出与成功实施，为更多高性能细晶压电陶瓷的设计及制备提供了可靠参考。
发明内容
本发明提供了一种具有晶界颗粒桥结构的高温细晶能量收集压电陶瓷及其制备方法。本发明的高温细晶压电陶瓷材料的特征在于具有晶界颗粒桥结构，即陶瓷晶界处存在规律性(如单列排布)排布的纳米级颗粒，且纳米颗粒与陶瓷晶粒内部具有协同的铁电畴。这种特殊晶界结构的存在使高温压电陶瓷材料在具有小晶粒尺寸的同时，保持良好的压电性能，进而实现高的换能系数，有利于作为高温压电能量收集材料使用。
为实现上述目的，本发明采取以下技术方案：
该高温压电陶瓷材料的化学组成为：0.345BiScO3-0.615PbTiO3-0.04Pb(In1/ 2Nb1/2)O3。
本发明上述具有晶界颗粒桥结构的高温细晶压电陶瓷材料的制备方法，其特征在于采用粒度分布均匀的纳米级前驱粉体，通过干压成型、无压烧结工艺获得目标陶瓷，具体包括以下步骤：
(1)将原料Bi2O3、TiO2、Sc2O3、Nb2O5、Pb3O4、In2O3置于烘箱中烘干12小时，按照化学计量比称量，以无水乙醇为介质进行12小时行星球磨，随后在120℃的条件下烘干，再于研钵中研细；
(2)研磨后的粉末进行90分钟、800转/分钟碳化钨高能球磨，随后将粉体研磨、过筛，将通过200目、未通过400目网筛的粉末于800MPa的压力下干压成型，获得素坯体；
(3)将素坯体于950℃烧结120分钟，获得目标陶瓷材料。
烧结后的陶瓷样品，经抛光处理后涂覆、烧结银电极，在30kV·cm-1的直流电场下人工极化，测试电学性能。
其中，0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3陶瓷的平均晶粒尺寸为0.26μm，其性能可达到：压电电荷常数d33＝343pC/N，换能系数d33×g33＝12274×10-15m2/N。
在本发明中，粉体经过球磨、过筛，粒径小，且粒度分布更为均匀。陶瓷晶界采用纳米颗粒填充形成特有的晶界颗粒桥结构，晶界中纳米颗粒(粒径约10nm左右)具备与陶瓷晶粒内部协同的铁电纳米畴，从而在人工极化时大幅降低外加电场作用下畴壁翻转受到的阻碍作用，提升极化效果，使得陶瓷在具有小晶粒尺寸的同时能够保持优异的压电性能，获得具有良好应用前景的高换能系数高温细晶能量收集压电陶瓷材料。
附图说明
图1为晶界颗粒桥结构设计策略图，(a)为该结构示意图，(b)为该结构对陶瓷性能提升作用示意图。
图2为本发明成分在950℃烧结的BS-PT-PIN陶瓷样品附图，(a)为陶瓷的断面扫描电镜(SEM)照片及晶粒尺寸分布图，可见细晶陶瓷平均晶粒尺寸为0.26μm，(b)为陶瓷晶界附近的高倍数透射电镜(TEM)图。由图可见陶瓷晶界含有规则排列的纳米颗粒，即形成晶界颗粒桥结构。
图3为本发明成分在950℃烧结的BS-PT-PIN陶瓷极化后样品的铁电畴附图。由图可见，晶界中纳米颗粒具备与陶瓷晶粒内部协同的铁电纳米畴。
图4为本发明成分不同温度烧结陶瓷极化后样品的铁电畴情况，(a)为900℃烧结，(b)为1000℃烧结，(c)为1050℃烧结。由图可见，样品不含晶界颗粒桥结构。因此，只有特定温度(950℃)烧结才可以获得具有协同畴的晶界颗粒桥结构。
具体实施方式
下面通过实施例进一步阐明本发明的实质性特点和显著优点。这些实施例只是出于示例性说明的目的，而非用于限定本发明。
实施例1：
将原料Bi2O3、TiO2、Sc2O3、Nb2O5、Pb3O4、In2O3置于烘箱中烘干12小时，按照化学式0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3称量，以150ml无水乙醇为介质进行12小时行星球磨，随后在120℃的条件下烘干，再于研钵中研细。研磨后的粉末进行90分钟、800转/分钟的碳化钨高能球磨，随后将粉体研磨、过筛，将通过200目、未通过400目网筛的粉末于800MPa的压力下干压成型，然后于950℃烧结120分钟，获得目标陶瓷材料。
对比例1：
按照化学式0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3称量原料Bi2O3、TiO2、Sc2O3、Nb2O5、Pb3O4、In2O3，烧结温度为900℃。其他同实施例1。
对比例2：
按照化学式0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3称量原料Bi2O3、TiO2、Sc2O3、Nb2O5、Pb3O4、In2O3，烧结温度为1000℃。其他同实施例1。
对比例3：
按照化学式0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3称量原料Bi2O3、TiO2、Sc2O3、Nb2O5、Pb3O4、In2O3，烧结温度为1050℃。其他同实施例1。
表1上述实施例性能对比表
Claims (2)
1.一种高温细晶能量收集压电陶瓷材料，其特征在于，陶瓷晶界处存在规律性排布的纳米级颗粒，且纳米颗粒与陶瓷晶粒内部具有协同的铁电畴；
该材料的化学组成为0.345BiScO3-0.615PbTiO3-0.04Pb(In1/2Nb1/2)O3；纳米颗粒粒径为10nm，陶瓷晶粒平均晶粒尺寸为0.26μm。
2.制备权利要求1所述的一种高温细晶能量收集压电陶瓷材料的制备方法，其特征在于，包括以下步骤：
(1)将原料Bi2O3、TiO2、Sc2O3、Nb2O5、Pb3O4、In2O3置于烘箱中烘干12小时，按照化学计量比称量，以150ml无水乙醇为介质进行12小时行星球磨，随后在120℃的条件下烘干，再于研钵中研细；
(2)研磨后的粉末进行90分钟、800转/分钟碳化钨高能球磨，随后将粉体研磨、过筛，将通过200目、未通过400目网筛的粉末于800MPa的压力下干压成型，获得素坯体；
(3)将素坯体于950℃烧结120分钟，获得目标陶瓷材料。
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