The Ni-, Co-, and Mo-supported Ni foam (NiF–NiCoMo) was produced via galvanostatic method, and electrooxidation of methanol in alkaline medium was examined. The characterization was achieved using field emission scanning electron microscopy, energy-dispersive X-ray, and X-ray diffraction analysis. The electrochemical behavior was determined via cyclic voltammetry and chronoamperometry analysis. The contribution of each transition metal to electrocatalytic performance of NiF was monitored via mono, binary, and ternary modifications of each transition metal (Ni, Co, and Mo) for several amounts (5, 10, and 15 μg). Experiments were performed to determine the influence of catalyst amounts, methanol concentration, and scan rate parameters. The impacts of independent parameters on methanol electrooxidation were statistically investigated using Design-Expert software. The ability to analyze multiple parameters with a limited number of experimental performances is one of the method’s key benefits. The developed model showed that 9.41 and 14.03 µg catalyst amounts were the appropriate values for NiF–NiMo and NiF–NiCoMo achieving optimal circumstances, respectively.