The Henry Royce Institute, Department of Materials, University of Manchester, M13 9PL, United Kingdom.
The Henry Royce Institute, Department of Materials, University of Manchester, M13 9PL, United Kingdom.
Ultramicroscopy. 2020 Jul;214:112989. doi: 10.1016/j.ultramic.2020.112989. Epub 2020 Apr 24.
Here we describe the first automated fully integrated in-microscope broad ion beam (BIB) system. Ar-BIB has several advantages over Ga focused ion beam (FIB) and Xe plasma-FIB (PFIB) methods inducing less beam damage, especially for ion beam sensitive materials. It can mill areas several orders of magnitude larger (up to millimetre scale), and is not confined to the edge of the sample with associated curtaining issues. BIB is shown to have sputter rates up to five times higher than comparable FIB techniques. This new coupled BIB-SEM system (commercial name 'iPrep™II') enables in-microscope surface polishing to remove contaminants or damage for two dimensional (2D) imaging, as well as automated serial section tomography (SST) by milling and imaging hundreds of slices, cost and time efficiently. The milled slice thickness can be controlled from a few nanometers up to a micrometre. A novel sample transfer, handling and interlock system allows automated and sequential BIB polishing, scanning electron microscopy (SEM) and analysis by secondary electron (SE) imaging, electron back scatter diffraction (EBSD) and energy dispersive spectroscopy (EDS) for 3D microstructure analysis. Furthermore, insulating surfaces can be sputter coated after milling each slice to reduce charging during SEM analysis. The performance of the instrument is demonstrated through a series of case studies across the materials, earth and life sciences exploiting the imaging, crystallographic and chemical mapping capabilities. These include the study of butterfly defects in bearing steels, meta-stable intermetallic phases in bronze bearings, shale gas rock, aluminium plasma electrolytic oxide (PEO) coatings as well as liver and mouse brain tissues.
在这里，我们描述了第一个全自动集成显微镜内宽束离子束（BIB）系统。与 Ga 聚焦离子束（FIB）和 Xe 等离子体 FIB（PFIB）方法相比，Ar-BIB 具有几个优势，特别是对离子束敏感的材料，它引起的束损伤更小。它可以铣削大几个数量级的区域（高达毫米尺度），并且不受与相关屏蔽问题相关的样品边缘限制。BIB 的溅射率比可比的 FIB 技术高 5 倍。这种新的耦合 BIB-SEM 系统（商业名称为 'iPrep™II'）能够在显微镜下进行表面抛光，以去除污染物或损坏，从而进行二维（2D）成像，以及通过铣削和成像数百个切片，高效地进行自动连续切片断层扫描（SST）。铣削片的厚度可以从几纳米到几微米进行控制。一种新颖的样品转移、处理和互锁系统允许自动化和顺序 BIB 抛光、扫描电子显微镜（SEM）和二次电子（SE）成像、电子背散射衍射（EBSD）和能量色散光谱（EDS）的分析，用于 3D 微观结构分析。此外，在铣削每个切片后，可以对绝缘表面进行溅射涂层，以减少 SEM 分析过程中的充电。该仪器的性能通过一系列跨越材料、地球和生命科学的案例研究得到了证明，这些研究利用了成像、晶体学和化学绘图能力。这些案例包括研究轴承钢中的蝴蝶缺陷、青铜轴承中的亚稳金属间化合物相、页岩气岩、铝等离子体电解氧化（PEO）涂层以及肝和鼠脑组织。
