Self-supported nickel antimonides/Ni architectured electrodes were prepared by solid state reaction from Ni thin film, Ni foam and Ni nanorods. This specific design is expected to optimize both NiSbx/Ni-current collector and NiSbx/electrolyte interfaces of the electrode in the Li ion battery. This new electrode preparation process is based on solid state reaction of antimony with the nickel architectured substrate. Preliminary electrochemical tests of the as-obtained self supported antimonide electrodes show improvement in the capacity retention of the NiSbx active material.