In this work, novel phosphate materials based on bimetallic character (Fe and Ni) were introduced by different chemical fabrication methods, the reflux method (FeNiP-R) and the sol-gel technique (FeNiP-S), and evaluated as non-precious electrodes for methanol electrooxidation in KOH electrolytes. The designed FeNiP-R and FeNiP-S samples were investigated using different characterization techniques, namely TEM, SEM, XPS, BET, DLS, and FT-IR, to describe the impact of the fabrication technique on the chemistry, morphology, and surface area. The characterization techniques indicate the successful fabrication of nanoscale-sized particles with higher agglomeration by the sol-gel technique compared with the reflux strategy. After that, the electrochemical efficiency of the fabricated FeNiP-R and FeNiP-S as electrodes for electrocatalytic methanol oxidation was studied through cyclic voltammetry (CV) at different methanol concentrations and scan rates in addition to impedance analysis and chronoamperometric techniques. From electrochemical analyses, a sharp improvement in the obtained current values was observed in both electrodes, FeNiP-R and FeNiP-S. During the MeOH electrooxidation over FeNiP-S, the current value was improved from 0.14 mA/cm2 at 0.402 V to 2.67 mA/cm2 at 0.619 V, which is around 109 times the current density value (0.0243 mA/cm2 at 0.62 V) found in the absence of MeOH. The designed FeNiP-R electrode showed an improved electrocatalytic character compared with FeNiP-S at different methanol concentrations up to 80 mmol/L. The enhancement of the anodic current density and charge transfer resistance indicates the methanol electrooxidation over the designed bimetallic Fe/Ni-phosphates.
