Electrocatalysis is an influential field in electrochemistry that has seen significant growth due to the application and ever-emerging synthetic techniques. The electrocatalytic ability of multi-walled carbon nanotubes (MWCNT) integrated with nanostructured materials has been a key area of research. These integrated nanohybrids are carefully architectured to produce complexes with new characteristics and properties that differ from their individual bulk components. These nanohybrids hold significance importance as they are used in various real world applications such as electrochemical reactions, organic electrosynthesis, fuel cells and battery preparation. This thesis aimed to investigate the characteristics and electrocatalytic parameters of 3 synthesised nanohybrids. The structures of the hybrids were revealed using microscopic techniques (performed by TEM, UV, Zeta potential and AFM). Electrochemical studies were performed by voltammetric and electrochemical techniques. The initial hybrid formed was AuNP on MWCNT (AuNP/MWCNT hybrid), however during the electrocatalytic analysis, the hybrid showed inconsistent results therefore no further investigations were performed.