The results of SPM-based localized electrical examination of precipitation hardened Waspaloy microstructures using Electrostatic Force Microscopy (EFM) and Current-Atomic Force Microscopy (I-AFM) are reported herein. The measurements were conducted on two differently etched specimens with the same initial microstructure. Selective etching by preferentially removing the γ′ or the γ phase resulted in a non-uniform surface topography leaving the less reactive phase standing in relief relative to the depressed phase. The presence of a non-uniform surface topography affected the measured EFM response by causing an inhomogeneous surface voltage distribution. A non-linear tip-surface interaction could have further complicated the measured EFM response by making it non-localized. The EFM phase obeyed a supplementary behavior upon reversing the polarity of the DC bias. Using I-AFM, the tip current was found to be the highest at γ-γ′ interphase boundaries, which was attributed to the relaxation of the lattice atoms in the relief zone formed upon etching.