In this paper, two failure analysis case studies are presented to demonstrate the importance of sample preparation procedures to successful failure analyses. Case study 1 establishes that Palladium (Pd) cannot be used as pre-FIB coating for SiO2 thickness measurement due to the spontaneously Pd silicide formation at the SiO2/Si interface. Platinum (Pt) is thus recommended, in spite of the Pt/SiO2 interface roughness, as the pre-FIB coating in this application. In the second case study, the dual-directional TEM inspection method is applied to characterize the profile of the “invisible” tungsten residue defect. The tungsten residue appears invisible in the planeview specimen due to the low mass-thickness contrast. It is then revealed in the cross-sectional TEM inspection.