Patel Binay, Watanabe Masashi
Department of Materials Science and Engineering, Lehigh University, Bethlehem, PA 18015, USA.
Microsc Microanal. 2014 Feb;20(1):124-32. doi: 10.1017/S1431927613014049. Epub 2014 Jan 15.
Scanning transmission electron microscopy in scanning electron microscopy (STEM-in-SEM) is a convenient technique for soft materials characterization. Various specimen-holder geometries and detector arrangements have been used for bright-field (BF) STEM-in-SEM imaging. In this study, to further the characterization potential of STEM-IN-SEM, a new specimen holder has been developed to facilitate direct detection of BF signals and indirect detection of dark-field (DF) signals without the need for substantial instrument modification. DF imaging is conducted with the use of a gold (Au)-coated copper (Cu) plate attached to the specimen holder which directs highly scattered transmitted electrons to an off-axis yttrium-aluminum-garnet (YAG) detector. A hole in the copper plate allows for BF imaging with a transmission electron (TE) detector. The inclusion of an Au-coated Cu plate enhanced DF signal intensity. Experiments validating the acquisition of true DF signals revealed that atomic number (Z) contrast may be achieved for materials with large lattice spacing. However, materials with small lattice spacing still exhibit diffraction contrast effects in this approach. The calculated theoretical fine probe size is 1.8 nm. At 30 kV, in this indirect approach, DF spatial resolution is limited to 3.2 nm as confirmed experimentally.
扫描电子显微镜中的扫描透射电子显微镜(STEM-in-SEM)是一种用于软材料表征的便捷技术。各种样品架几何形状和探测器配置已被用于明场(BF)STEM-in-SEM成像。在本研究中,为了进一步拓展STEM-in-SEM的表征潜力,开发了一种新的样品架,无需对仪器进行大量修改即可直接检测BF信号并间接检测暗场(DF)信号。DF成像通过使用附着在样品架上的镀金(Au)铜板进行,该铜板将高度散射的透射电子导向离轴钇铝石榴石(YAG)探测器。铜板上的一个孔允许使用透射电子(TE)探测器进行BF成像。镀金铜板的加入增强了DF信号强度。验证获取真实DF信号的实验表明,对于具有大晶格间距的材料可以实现原子序数(Z)对比度。然而,在这种方法中,具有小晶格间距的材料仍然表现出衍射对比度效应。计算得到的理论精细探针尺寸为1.8 nm。在30 kV下,通过实验证实,在这种间接方法中,DF空间分辨率限制为3.2 nm。