Padgett Elliot, Hovden Robert, DaSilva Jessica C, Levin Barnaby D A, Grazul John L, Hanrath Tobias, Muller David A
1School of Applied and Engineering Physics,Cornell University,Ithaca,NY 14853,USA.
3School of Chemical and Biomolecular Engineering,Cornell University,Ithaca,NY 14853,USA.
Microsc Microanal. 2017 Dec;23(6):1150-1158. doi: 10.1017/S1431927617012764. Epub 2017 Dec 11.
Electron tomography has become a valuable and widely used tool for studying the three-dimensional nanostructure of materials and biological specimens. However, the incomplete tilt range provided by conventional sample holders limits the fidelity and quantitative interpretability of tomographic images by leaving a "missing wedge" of unknown information in Fourier space. Imaging over a complete range of angles eliminates missing wedge artifacts and dramatically improves tomogram quality. Full-range tomography is usually accomplished using needle-shaped samples milled from bulk material with focused ion beams, but versatile specimen preparation methods for nanoparticles and other fine powders are lacking. In this work, we present a new preparation technique in which powder specimens are supported on carbon nanofibers that extend beyond the end of a tungsten needle. Using this approach, we produced tomograms of platinum fuel cell catalysts and gold-decorated strontium titanate photocatalyst specimens. Without the missing wedge, these tomograms are free from elongation artifacts, supporting straightforward automatic segmentation and quantitative analysis of key materials properties such as void size and connectivity, and surface area and curvature. This approach may be generalized to other samples that can be dispersed in liquids, such as biological structures, creating new opportunities for high-quality electron tomography across disciplines.
电子断层扫描已成为研究材料和生物样本三维纳米结构的一种有价值且广泛使用的工具。然而,传统样品架提供的倾斜范围不完整,在傅里叶空间中留下未知信息的“缺失楔形”,限制了断层图像的保真度和定量解释性。在完整角度范围内成像可消除缺失楔形伪影,并显著提高断层图像质量。全范围断层扫描通常使用聚焦离子束从块状材料中铣削出的针状样品来完成,但缺乏适用于纳米颗粒和其他细粉的通用样品制备方法。在这项工作中,我们提出了一种新的制备技术,其中粉末样品支撑在延伸到钨针末端之外的碳纳米纤维上。使用这种方法,我们制作了铂燃料电池催化剂和金修饰钛酸锶光催化剂样品的断层图像。没有缺失楔形,这些断层图像没有伸长伪影,支持对关键材料特性(如孔隙尺寸和连通性、表面积和曲率)进行直接的自动分割和定量分析。这种方法可以推广到其他可分散在液体中的样品,如生物结构,为跨学科的高质量电子断层扫描创造新机会。