Electrocatalytic Properties of Pulse-Reverse Electrodeposited Nickel Phosphide for Hydrogen Evolution Reaction

Nickel phosphide (Ni-P) films as a catalytic cathode for the hydrogen evolution reaction (HER) of a water splitting were fabricated by a pulse-reverse electrodeposition technique. The electrochemical behaviors for the electrodeposition of Ni-P were investigated by the characterization of peaks in a cyclic voltammogram. The composition of the electrodeposited Ni-P alloys was controlled by adjusting duty cycles of the pulse-reverse electrodeposition. The HER electrocatalytic properties of the Ni-P electrodeposits with an amorphous phase as a function of phosphorous contents existing in Ni-P were electrochemically characterized by the analysis of overpotentials, Tafel slopes, and electrochemical impedance spectrometry. Additionally, the elemental Ni-embedded crystalline Ni₃P was prepared by an annealing process with the amorphous Ni₆₉P₃₁ electrodeposit with high contents of phosphorus. The crystalline structure with Ni inclusions in the matrix of Ni₃P was formed by the precipitation of excess Ni. The electrocatalytic properties of crystalline Ni₃P with elemental Ni inclusions were also investigated by electrochemical characterization.