Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA.
Microsc Microanal. 2012 Dec;18(6):1410-8. doi: 10.1017/S1431927612013517. Epub 2012 Nov 12.
A sample preparation method is described for enabling direct correlation of site-specific plan-view and cross-sectional transmission electron microscopy (TEM) analysis of individual nanostructures by employing a dual-beam focused-ion beam (FIB) microscope. This technique is demonstrated using Si nanowires dispersed on a TEM sample support (lacey carbon or Si-nitride). Individual nanowires are first imaged in the plan-view orientation to identify a region of interest; in this case, impurity atoms distributed at crystalline defects that require further investigation in the cross-sectional orientation. Subsequently, the region of interest is capped with a series of ex situ and in situ deposited layers to protect the nanowire and facilitate site-specific lift-out and cross-sectioning using a dual-beam FIB microscope. The lift-out specimen is thinned to electron transparency with site-specific positioning to within ≈ 200 nm of a target position along the length of the nanowire. Using the described technique, it is possible to produce correlated plan-view and cross-sectional view lattice-resolved TEM images that enable a quasi-3D analysis of crystalline defect structures in a specific nanowire. While the current study is focused on nanowires, the procedure described herein is general for any electron-transparent sample and is broadly applicable for many nanostructures, such as nanowires, nanoparticles, patterned thin films, and devices.
介绍了一种样品制备方法,通过采用双束聚焦离子束(FIB)显微镜,能够实现对单个纳米结构的局域平面视图和横截面透射电子显微镜(TEM)分析的直接关联。该技术使用分散在 TEM 样品支撑物(网格碳或氮化硅)上的 Si 纳米线进行了演示。首先在平面视图方向上对各个纳米线进行成像,以识别感兴趣的区域;在这种情况下,杂质原子分布在需要在横截面方向进一步研究的晶体缺陷处。随后,用一系列原位和异位沉积层覆盖感兴趣的区域,以保护纳米线并便于使用双束 FIB 显微镜进行特定位置的取出和截面处理。使用特定位置的取出样本减薄至电子透明性,在纳米线长度方向上与目标位置的距离约为 200nm。通过描述的技术,可以产生相关的平面视图和横截面视图晶格分辨 TEM 图像,从而能够对特定纳米线中的晶体缺陷结构进行准 3D 分析。虽然当前的研究集中在纳米线上,但本文描述的程序适用于任何电子透明的样品,并且广泛适用于许多纳米结构,如纳米线、纳米粒子、图案化薄膜和器件。