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Synergy between transmission electron microscopy and powder diffraction: application to modulated structures

机译:透射电子显微镜与粉末衍射之间的协同作用:在调制结构中的应用

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摘要

The crystal structure solution of modulated compounds is often very challenging, even using the well established methodology of single-crystal Xray crystallography. This task becomes even more difficult for materials that cannot be prepared in a single-crystal form, so that only polycrystalline powders are available. This paper illustrates that the combined application of transmission electron microscopy (TEM) and powder diffraction is a possible solution to the problem. Using examples of anion-deficient perovskites modulated by periodic crystallographic shear planes, it is demonstrated what kind of local structural information can be obtained using various TEM techniques and how this information can be implemented in the crystal structure refinement against the powder diffraction data. The following TEMmethods are discussed: electron diffraction (selected area electron diffraction, precession electron diffraction), imaging (conventional high-resolution TEM imaging, highangle annular dark-field and annular bright-field scanning transmission electron microscopy) and state-of-the-art spectroscopic techniques (atomic resolution mapping using energy-dispersive X-ray analysis and electron energy loss spectroscopy).
机译:即使使用成熟的单晶X射线晶体学方法,调制化合物的晶体结构解决方案通常也非常具有挑战性。对于不能以单晶形式制备的材料,该任务变得更加困难,因此只能使用多晶粉末。本文说明,透射电子显微镜(TEM)和粉末衍射的组合应用可能是解决该问题的方法。使用通过周期性晶体剪切面调制的阴离子不足钙钛矿的例子,证明了使用各种TEM技术可以获得什么样的局部结构信息,以及如何在针对粉末衍射数据的晶体结构细化中实现该信息。讨论了以下TEM方法:电子衍射(选择区域电子衍射,进动电子衍射),成像(常规高分辨率TEM成像,高角度环形暗场和环形明场扫描透射电子显微镜)和最新技术光谱技术(使用能量色散X射线分析和电子能量损失光谱的原子分辨率制图)。

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