A method for making a metal oxyhydroxide electrocatalytic material comprises titrating a precursor solution with a (bi)carbonate salt, the precursor solution comprising a first metal salt and a solvent, wherein the titration induces reactions between the (bi)carbonate salt and the first metal salt to provide first metal carbonate species in the titrated precursor solution; and exposing the titrated precursor solution to microwave radiation to decompose the first metal carbonate species to form the metal oxyhydroxide electrocatalytic material and carbon dioxide. Mixed metal oxyhydroxide electrocatalytic materials such as nickel-iron oxyhydroxide may be formed. Also provided are the materials themselves, electrocatalytic systems comprising the materials, and methods of using the materials and systems.