近日，瑞士苏黎世联邦理工学院的Andreas Apseros&Valerio Scagnoli与日本广岛大学的Claire Donnelly等人合作并取得一项新进展。他们实现了晶体和拓扑缺陷的X射线线性二向色层析成像。相关研究成果已于2024年12月11日在国际权威学术期刊《自然》上发表。

据悉，材料的功能由其成分和微观结构决定，即晶粒的分布和取向、晶界以及晶界内的缺陷。迄今为止，用于绘制晶粒分布、晶粒取向以及缺陷存在的表征技术仅限于表面研究、几百纳米的空间分辨率或约100纳米厚度的系统，因此需要进行破坏性的样品制备才能进行测量，这阻碍了对系统代表性体积的研究或在运行条件下对材料的研究。

该研究团队提出一种名为X射线线性二向色性取向断层成像（XL-DOT）的定量、非侵入式技术，该技术能够在三维空间内对扩展的多晶和非晶材料进行晶内和晶间表征。研究人员以生产硫酸过程中的关键催化剂五氧化二钒（V₂O₅）的多晶样品为例，进行了详细表征。

研究人员以73纳米的空间分辨率确定了整个多晶样品的纳米级成分、微观结构和晶体取向。研究人员识别并表征了晶粒，以及扭转、倾斜和孪晶晶界。他们还进一步观察了由体积晶体学缺陷引起的拓扑缺陷的产生和湮灭。这一方法具有非破坏性和光谱分析的特性，为在运行状态下对功能材料（包括能源材料、机械材料和量子材料），进行化学和微观结构的组合研究打开了大门。

附：英文原文

Title: X-ray linear dichroic tomography of crystallographic and topological defects

Author: Apseros, Andreas, Scagnoli, Valerio, Holler, Mirko, Guizar-Sicairos, Manuel, Gao, Zirui, Appel, Christian, Heyderman, Laura J., Donnelly, Claire, Ihli, Johannes

Issue&Volume: 2024-12-11

Abstract: The functionality of materials is determined by their composition and microstructure, that is, the distribution and orientation of crystalline grains, grain boundaries and the defects within them. Until now, characterization techniques that map the distribution of grains, their orientation and the presence of defects have been limited to surface investigations, to spatial resolutions of a few hundred nanometres or to systems of thickness around 100nm, thus requiring destructive sample preparation for measurements and preventing the study of system-representative volumes or the investigation of materials under operational conditions. Here we present X-ray linear dichroic orientation tomography (XL-DOT), a quantitative, non-invasive technique that allows for an intragranular and intergranular characterization of extended polycrystalline and non-crystalline materials in three dimensions. We present the detailed characterization of a polycrystalline sample of vanadium pentoxide (V₂O₅), a key catalyst in the production of sulfuric acid. We determine the nanoscale composition, microstructure and crystal orientation throughout the polycrystalline sample with 73nm spatial resolution. We identify and characterize grains, as well as twist, tilt and twin grain boundaries. We further observe the creation and annihilation of topological defects promoted by the presence of volume crystallographic defects. The non-destructive and spectroscopic nature of our method opens the door to operando combined chemical and microstructural investigationsof functional materials, including energy, mechanical and quantum materials.

DOI: 10.1038/s41586-024-08233-y

Source: https://www.nature.com/articles/s41586-024-08233-y