The influence of varying the Ar-pressure in the process of depositing Ni/C multilayers by DC-magnetron sputtering has been studied, and Atomic Force Microscopy (AFM) measurements, X-ray characterization results and Transmission Electron Microscopy (TEM) results are presented. Single Ni and C films and Ni/C multilayers were deposited at Ar-pressures of 1.5, 3, 5 and 7 mTorr. The one-dimensional power spectral density data from the AFM measurements clearly indicate that the best densities and film qualities for both materials are obtained at lower Ar-pressures, i.e. 1.5 mTorr.