一种对亚微米大小的粒子进行全倾斜角电子断层扫描的实用方法

IF 2.2 3区工程技术 Q1 MICROSCOPY

Micron Pub Date : 2025-07-02 DOI:10.1016/j.micron.2025.103874

Jun Yamasaki , Tomohito Ishii , Kaito Teruya , Yuya Ubata , Hiroya Miyazaki , Keita Kobayashi , Takeharu Kato

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引用次数: 0

摘要

在这项研究中，开发了一种实用的方法来进行全倾角电子断层扫描颗粒尺寸为几个100纳米。为了实现这一目标，我们设计了一个用于200千伏透射电子显微镜（TEM）的样品架，并设计了一种方案，可以在配备扫描电子显微镜（SEM）的聚焦离子束（FIB）仪器中拾取感兴趣的粒子。在该方案中，碳沉积通过电子束被用来将颗粒附着在钨针的尖端。该技术防止了镓离子束的表面腐蚀和辐射引起的损伤，并确保了清晰的TEM观测。随后，将W针从FIB-SEM系统中分离出来，固定在已开发的标本夹上。通过测角仪，在TEM中，即使使用具有极片的物镜，也可以将支架倾斜±90°以获得原子分辨率。通过采用该方法，本研究使用聚苯乙烯乳胶颗粒的TEM图像和ZnO四足体颗粒的环形暗场扫描TEM图像证明了全倾斜角度断层扫描。这些亚微米大小的颗粒的外部形状得到了清晰的三维（3D）重建，没有丢失的楔形效应。通过小心地将这些粒子放置在中心轴上，可以在- 90°和+ 90°之间获得用于断层扫描的倾斜序列，而无需对倾斜引起的移位进行位置补偿。利用这一优势，实现了亚微米尺寸ZnO粒子的全倾角快速层析成像。基于在连续倾斜过程中记录的25秒电影，我们实现了与传统断层扫描质量相似的3D重建，其中测量进行了一个多小时。通过原子分辨率的侧视图观察附着在W针上的粒子的机械稳定性，使用附加的倾斜机构集成到开发的支架中。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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A practical method for performing full-tilt-angle electron tomography of submicron-sized particles

In this study, a practical method for performing full-tilt-angle electron tomography for particles with sizes of several 100 nanometers was developed. To achieve this, we designed a specimen holder for a 200-kV transmission electron microscope (TEM) and a protocol that can pick up the particle of interest in a focused ion beam (FIB) instrument equipped with a scanning electron microscope (SEM). In the protocol, carbon deposition through electron beams was used to attach the particle to the tip of a tungsten (W) needle. This technique prevents surface etching and radiation-induced damage by Ga ion beams and ensures clear TEM observations. Subsequently, the W needle was detached from the FIB–SEM system and fixed to the developed specimen holder. The holder can be tilted by ±90° in a TEM through a goniometer, even with an objective lens having a pole piece with a narrow gap for atomic resolution. By employing this procedure, full-tilt-angle tomography was demonstrated in this study using TEM images of a polystyrene latex particle and annular dark-field scanning TEM images of a ZnO tetrapod particle. Clear three-dimensional (3D) reconstructions of the external shapes of these submicron-sized particles were obtained without the missing wedge effect. By carefully placing these particles on the eucentric axis, a tilt series for tomography is obtained between −90° and + 90° without position compensation against the shifts induced by tilting. Using this advantage, full-tilt-angle fast tomography of submicron-sized ZnO particles was achieved. Based on a 25-s movie recorded during continuous tilting, we realized 3D reconstruction having a quality similar to that of conventional tomography, where the measurement is performed for over more than an hour. The mechanical stability of a particle attached to the W needle was assessed through atomic-resolution side-view observation of a plate-like flake of TiSe₂ using an additional tilting mechanism incorporated into the developed holder.

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来源期刊

Micron 工程技术-显微镜技术

CiteScore

4.30

自引率

4.20%

发文量

100

审稿时长

31 days

期刊介绍： Micron is an interdisciplinary forum for all work that involves new applications of microscopy or where advanced microscopy plays a central role. The journal will publish on the design, methods, application, practice or theory of microscopy and microanalysis, including reports on optical, electron-beam, X-ray microtomography, and scanning-probe systems. It also aims at the regular publication of review papers, short communications, as well as thematic issues on contemporary developments in microscopy and microanalysis. The journal embraces original research in which microscopy has contributed significantly to knowledge in biology, life science, nanoscience and nanotechnology, materials science and engineering.