Toward 3D imaging of corrosion at the nanoscale: Cross-sectional analysis of in-situ oxidized TEM samples.

Understanding the effect of microstructural features on corrosion behavior will allow for significant improvements to alloy design for harsh environments. Recently, in-situ TEM has been recognized to offer significant data on corrosion behavior at the nanoscale, but in order for the best information to be acquired, a three dimensional view of the oxidation process is needed so that oxide structure and phase can be identified. Described herein is a new method of sample preparation for transmission electron microscopy (TEM) using a focused ion beam (FIB) to cross-section a previously FIB prepared sample. In-situ TEM was used to oxidize a sample using an environmental cell, and this in-situ sample is cross-sectioned to study oxide depth and oxide structure. This technique provides a new method to investigate in-situ TEM samples in 3D.