3D Volume Microscopy and TEM Sample Preparation of Complex Hybrid Nanostructures

在双光束中使用聚焦离子束（FIB），分析扫描电子显微镜（SEM）对固体进行连续离子束切片，可以在数百立方微米的体积上研究三维（3D）化学微观和纳米结构，即所谓的3D体积显微镜，其分辨率高于使用x射线微断层扫描所能达到的分辨率。此外，还可以提取特定位点的薄透射电子显微镜（TEM）横截面，以便对微观结构内的表面或界面进行更高分辨率的分析。液氮冷却样品低温级的使用减少了离子束损伤，并允许应用于光束敏感样品，如无机-有机混合材料，有机物和冷冻样品，否则极具挑战性。此外，包含一个冷却的纳米机械手和一个扫描TEM （STEM）探测器，可以对冷冻的TEM薄片进行原位成像，原则上，可以将冷冻转移到外部冷冻TEM进行额外的分析。除了减少传统无机材料的损伤外，这种能力还为复杂软固体（以及潜在的液体分散体）的表征开辟了新的视野，这些固体被广泛用于医疗、化学、结构和电子应用。

Use of a focused ion beam (FIB) in a dual beam, analytical scanning electron microscope (SEM) for serial ion beam sectioning of solids allows the investigation of the three dimensional (3D) chemical micro- and nanostructure over volumes of hundreds of cubic microns, so called 3D volume microscopy, at resolutions greater than that achievable using X-ray microtomography. In addition, it is possible to extract site-specific thin transmission electron microscopy (TEM) cross-sections for the higher resolution analysis of surfaces or interfaces within the microstructure. The use of a liquid nitrogen-cooled sample cryo-stage reduces ion beam damage and permits the application to beam-sensitive samples such as hybrid inorganic-organic materials, organics and also frozen samples which is otherwise extremely challenging. Furthermore, the inclusion of a cooled nanomanipulator and a scanning TEM (STEM) detector enables in-situ imaging of frozen TEM lamella that, in principle, could be cryo-transferred to an external cryo-TEM for additional analysis. As well as reducing damage in conventional inorganic materials, such a capability opens up new horizons for the characterisation of complex soft solids (and potentially liquid dispersions) used in a wide range of medical, chemical, structural and electronic applications.