Microstructural characterization of thin alumina scales formed on oxidized Ni-base alloys using transmission electron microscopy (TEM) has long been a challenge as a result of the many problems encountered during the preparation of thin specimens. Successful and reproducible preparation of uniformly thin, cross-section TEM specimens from these multicomponent “layered” structures (alumina scale on a metallic substrate) is extremely difficult using standard ion beam thinning procedures for several reasons: (1) differential thinning of the various constituents in the system can occur, (2) a weak ceramic-metal interface may lead to separation during the harsh mechanical grinding and thinning procedure, (3) fully intact scales are rarely achieved since native surface structures are usually lost during ion milling, and (4) extensive damage can be created in the scale and alloy during rough grinding and polishing steps as well as during final ion beam thinning.