Ni-La electrocatalytic systems have been synthesized via spray pyrolysis and studied for the electrooxidation of hydrazine hydrate in alkaline media. Characterization of phase compositions, crystal structures, morphologies, and surface compositions of the electrocatalysts performed via XRD, SEM, HRTEM, and XPS in combination with in situ IRRAS spectroelectrochemistry permitted the further understanding of the high electrochemical activity obtained from Ni-La (lanthanum hydroxide) catalytic systems. Ni0.90La0.10 and Ni0.95La0.05 have been identified as highly active electrocatalysts for the oxidation of hydrazine hydrate demonstrating to be promising candidates as anodes in direct hydrazine alkaline anion-exchange membrane fuel cells (DHAFC).