Abstract: Gold nanostructures such as nanoparticles, nanowires, or nanotubes are highly preferred structures in electrochemical studies and can be produced by electrodeposition. This study points out that the shapes and electrochemical behaviour of electrodeposited gold nanostructures can be varied by adjusting multi-walled carbon nanotube (MWCNT) ratio in electrodeposition solution. For that, gold nanofilms on the glassy carbon electrode surface were formed from HAuCl4 solution in the presence and absence of MWCNT. In this study, the gold concentration was fixed at 0.4 ppm (10.0 mM) and only MWCNT concentration was varied. The prepared electrode surfaces were characterized and compared with each other from the point of view of electrochemical, microscopic, and spectroscopic properties. Ultimately, it was shown that each prepared electrode had different properties. Graphic abstract: [Figure not available: see fulltext.]