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

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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.