**Abstract**

This book chapter reports on various catalyst synthesis methods (impregnation, polyol, modified polyol, and microwave-assisted modified polyol methods) to determine which method would result in the most electrochemically active platinumruthenium (PtRu) electrocatalyst supported on multi-walled carbon nanotubes (MWCNTs) for methanol oxidation reaction in an acidic medium. Different techniques were used to characterize the synthesized catalysts, including the highresolution transmission electron microscope used for morphology and calculating particle sizes, and X-ray diffraction for determining crystalline sizes. The electroactive catalyst surface area, ECSA of the electrocatalysts was determined using cyclic voltammetry (CV), while the electroactivity, electron kinetics, and stability of the electrocatalysts towards methanol oxidation were evaluated using CV, electrochemical impedance spectroscopy, and chronoamperometry, respectively. The microwaveassisted modified polyol method produced the PtRu/MWCNT electrocatalyst with the most enhanced electrocatalytic activity compared to other PtRu/MWCNT catalysts produced by the impregnation, polyol, and modified polyol methods.

**Keywords:** methanol oxidation, catalysts, multi-walled carbon nanotubes, electrocatalytic activity
