This book describes the preparation and characterization of nickel dispersed polyaniline matrix. Electronically conducting polyaniline was made magnetic in nature by incorporating magnetic metals into its matrix. In this connection, metallic Ni particles were successfully dispersed onto polyaniline matrix by a simple one step electrochemical method. Polyaniline/Ni film matrix as prepared was found to have excellent electroactivity. The result based on cyclic voltammogram suggests a better electrochemical stability of the polyaniline/Ni electrode relative to the bulk polyaniline film. An energy dispersed X-ray analysis showed a Ni content of approximately 4.26% in the polyaniline matrix.The electrical conductivity measurements showed the conductivity of PANI and PANI/NI in order of 10-3 and 10-7 Scm-1. The Ni particles that incorporated into the polymer matrix may create blockage in the conductance for the PANI/Ni matrix. The sign of the susceptibility values clearly indicates that PANI is diamagnetic in nature whereas PAN/Ni is paramagnetic one. Compared to PANI, PANI/Ni film electrode was also found to provide a superior stability on its degradation at highly positive potential.