On the Microanalysis of Small Precipitates at Low Voltage with a FE-SEM

Abstract

The observation of microstructural features smaller than 300 nm is generally performed using Transmission Electron Microscopy (TEM) because conventional Scanning Electron Microscopes (SEM) do not have the resolution to image such small phases. Since the early 1990’s, a new generation of microscopes is now available on the market. These are the Field Emission Gun Scanning Electron Microscope with a virtual secondary electron detector. The field emission gun gives a higher brightness than those obtained using conventional electron filaments allowing enough electrons to be collected to operate the microscope with incident electron energy, E0, below 5 keV, with probe diameter smaller than 2.5 nm. Furthermore, what gives FE-SEM outstanding resolution is the combination of new magnetic lenses with a virtual secondary electron (SE) detector. The new lenses are designed to reduce the spherical and chromatic aberration coefficients, giving a smaller probe size. Contrary to the conventional systems, the SE detector is located above the objective lens and it becomes a virtual or through-the-lens (TTL) detector. Therefore, the SE image is mostly made up of all SEs of type I, almost eliminating those of type II and III which are generated by the backscattered electrons inside the specimen as well as in the chamber. It has been shown recently that Nb(CN) precipitates in Fe, as small than 10 nm, can be imaged with a FE-SEM Hitachi S-4500 with the TTL detector.