In this study, amorphous Ni-P films were deposited by electroless plating under different pH values. Their mechanical properties and deformation behavior were then investigated by instrumented nanoindentation. With increasing pH value of the plating solution from 3.75 to 6.0, the hardness and elastic modulus of the obtained Ni-P films increased from 6.1 GPa and 146 GPa to 8.2 GPa and 168 GPa respectively. From the load-indentation depth curve, the Ni-P films were found to yield at an indentation depth of 8 nm. By microstructural examination around the indented regions, early-stage plastic deformation of the amorphous Ni-P films was verified through the formation and extension of shear bands with a spacing of several tens of nanometers. Within the shear bands, flow dilatationinduced intense shear localization was expected and resulted in crystallization in the amorphous matrix. The critical shear stress and energy release rate required for the initiation of early-stage plastic yielding of the Ni-P films were calculated to be about 1.4 GPa and 3.0 J/m(2) respectively, both of which increased with pH values