This work concerned with preparation of Carbon Nitride thin films which is theoretically compete Diamond in hardness. CNx films perpared by the electrolysis of methanol -urea organic solution under different concentrations and applied voltages. This study characterized the structure of the prepared films by FTIR and GIXRD techniques and studied the optical properties of the CNx films by UV-Vis spectrometer. this study aimed at how the nitrogen to carbon ratio in the deposited films affect the structure and the properties of the deposited films.