A series of novel carbon nanofibers (CNFs) supported bimetallic copper/zirconia catalysts are synthesized by deposition precipitation method and calcined at different temperatures. Calcined catalysts are characterized by various techniques like X-ray diffraction, N sub(2) adsorption-desorption, N sub(2)O chemisorption, high resolution transmission electron microscopy, temperature programmed reduction, X-ray photo-electron spectroscopy and temperature programmed desorption (CO sub(2) & NH sub(3)). The structure-activity correlation is discussed in details. The results demonstrate 450 degreesC as optimum calcination temperature for methanol synthesis rate with CO sub(2)/H sub(2) feed volume ratio of 1:3. CO sub(2) conversion is found to be directly proportional to copper metallic surface area (S sub(Cu)), while a linear relationship is observed between methanol synthesis rate and fraction of dispersed Cu.