A method of making an electrode structure is provided. The method includes disposing an electrocatalytic material on an electrode, applying heat to the electrocatalytic material to form a volatile oxide of the electrocatalytic material, and applying a voltage to the electrode to reduce the volatile oxide to provide a number of nano-sized electrocatalytic particles on or proximate to a triple phase boundary, where the number of nano-sized electrocatalytic particles is greater on or proximate to the triple phase boundary than in an area that is not on or proximate to the triple phase boundary, and where the triple phase boundary is disposed on the electrode.