Moore K, Conroy M, Bangert U
Department of Physics, Bernal Institute, University of Limerick, Limerick, Ireland.
J Microsc. 2020 Sep;279(3):222-228. doi: 10.1111/jmi.12876. Epub 2020 Feb 21.
Ferroelectric materials, and more specifically ferroelectric domain walls (DWs) have become an area of intense research in recent years. Novel physical phenomena have been discovered at these nanoscale topological polarization discontinuities by mapping out the polarization in each atomic unit cell around the DW in a scanning transmission electron microscope (STEM). However, identifying these features requires an understanding of the polarization in the overall domain structure of the TEM sample, which is often a time-consuming process. Here, a fast method of polarization mapping in the TEM is presented, which can be applied to a range of ferroelectric materials. Due to the coupling of polarization to spontaneous strain, we can isolate different strain states and demonstrate the fast mapping of the domain structure in ferroelectric lead titanate (PTO). The method only requires a high-resolution TEM or STEM image and is less sensitive to zone axis or local strain effects, which may affect other techniques. Thus, it is easily applicable to in-situ experiments. The complimentary benefits of Fourier masking with more advanced mapping strategies and its application to other materials are discussed. These results imply that Fourier masked polarization mapping will be a useful tool for electron microscopists in streamlining their analysis of ferroelectric TEM samples. LAY DESCRIPTION: This paper addresses a problem that often occurs when looking at a ferroelectric material in the Transmission Electron Microscope (TEM). Ferroelectric samples are interesting because they form tiny areas inside themselves with arrow of charge in each one. The thinner the sample, the smaller these regions, called "domains" become. These arrows of charge point in different directions in each domain of the sample. The boundary where these domains meet have interesting properties to study in a TEM but it's important to figure out which way the arrows point in the domains around the boundary. What causes the arrows in the different domains is tiny shifts of different atoms in unit cell away from their neutral position, usually because they're being squeezed by pressure from the domains nearby. The problem is that these tiny atoms moving are difficult to measure and see where the charged arrow is pointing, often it's hard to know how many different domains are even in the sample and where they begin. This paper discusses a method called "Fourier masking" to quickly see what's going on in the overall TEM sample, where the domains are and roughly where the arrows point. It does this by looking at the spacings of the atoms from a magnification where you can just about see the lines of atoms. In lead titanate the unit cell is a rectangle and the arrow always points in line with the long side of the rectangle. The Fourier masking lets you see which direction the long side of the rectangular unit cell is pointing in different parts of your TEM image. The big advantage is that it takes about two minutes to do and uses software that almost every TEM already has. That lets the TEM user quickly know where the domains are in their TEM samples and roughly which way the arrows of charge are pointing. Then they can choose the most interesting features focus on for higher resolution analysis.
近年来,铁电材料,尤其是铁电畴壁,已成为一个热门的研究领域。通过在扫描透射电子显微镜(STEM)中绘制畴壁周围每个原子晶胞中的极化情况,人们在这些纳米级拓扑极化不连续处发现了新的物理现象。然而,识别这些特征需要了解透射电子显微镜(TEM)样品整体畴结构中的极化情况,这通常是一个耗时的过程。本文提出了一种在TEM中进行极化映射的快速方法,该方法可应用于一系列铁电材料。由于极化与自发应变的耦合,我们可以分离出不同的应变状态,并展示了铁电钛酸铅(PTO)中畴结构的快速映射。该方法仅需要高分辨率TEM或STEM图像,并且对可能影响其他技术的晶带轴或局部应变效应不太敏感。因此,它很容易应用于原位实验。本文还讨论了傅里叶掩蔽与更先进映射策略的互补优势及其在其他材料中的应用。这些结果表明,傅里叶掩蔽极化映射将成为电子显微镜学家简化铁电TEM样品分析的有用工具。通俗解释:本文解决了在透射电子显微镜(TEM)中观察铁电材料时经常出现的一个问题。铁电样品很有趣,因为它们内部会形成微小区域,每个区域都有电荷箭头。样品越薄,这些称为“畴”的区域就越小。样品每个畴中的电荷箭头指向不同方向。这些畴相遇的边界在TEM中有有趣的性质可供研究,但弄清楚边界周围畴中箭头的指向很重要。不同畴中箭头的形成是由于晶胞中不同原子从其中性位置发生微小位移,通常是因为它们受到附近畴的压力挤压。问题在于这些微小原子的移动很难测量,也很难看出带电箭头指向何处,通常很难知道样品中甚至有多少个不同的畴以及它们从哪里开始。本文讨论了一种称为“傅里叶掩蔽”的方法,用于快速了解TEM样品整体的情况,畴在哪里以及箭头大致指向哪里。它通过从一个能勉强看到原子排列的放大倍数下观察原子间距来实现。在钛酸铅中,晶胞是矩形的,箭头总是与矩形的长边方向一致。傅里叶掩蔽能让你在TEM图像的不同部分看到矩形晶胞长边的指向。最大的优势是大约两分钟就能完成,并且使用的软件几乎每个TEM都有。这能让TEM用户快速知道他们样品中的畴在哪里,以及电荷箭头大致指向哪个方向。然后他们可以选择最感兴趣的特征进行更高分辨率的分析。