Ni-Ti surface alloy was prepared by ion-implanting Ni into Ti. The surface film was amorphous having a Ni surface content of 10–40 at.%. The material was compared with a Ni-Ti bulk alloy (44.08:55.9) regarding their redox and electrocatalytic behavior in NaOH by cyclic voltammetry. The surface was characterized by x-ray photoelectron spectroscopy, x-ray and electron diffraction, transmission electron microscopy, and atomic force microscopy. The ion-implanted material revealed an enhanced activity toward the redox conversion of Ni(OH)2 ↔ NiOOH and the anodic oxidation of glucose. The effect is discussed considering the enhanced generation of active Ni surface sites from amorphous Ni and the stabilization of higher valence Ni by Ti.