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Nickel films of 40 nm thickness were obtained by means of magnetron sputtering on a single-crystalline silicon substrate. The films were subjected to rapid thermal treatment (RTT) for 7 s until the temperature increased from 200 to 550 °C. By means of the X-ray diffraction method, the structural-phase composition of nickel films before and after RTT was explored. The atomic force microscopy method due to direct contact with the surface under study, made it possible to accurately define the microstructure, roughness, specific surface energy and grain size of the nickel films before and after RTT, as well as to establish the relationship of these parameters with the phase composition and electrical properties of the films. Surface specific resistance was measured using the four-probe method. Based on XRD results, formation of Ni2Si and NiSi phases in the film was ascertained after RTT at 300 °C. At RTT 350–550 °C, only the NiSi phase was formed in the film. The microstructure and grain size significantly depend on the phase composition of the films. A correlation has been established between specific surface energy and resistivity with the average grain size after RTT at 350–550 °C, which is associated with the formation and constant restructuring of the crystal structure of the NiSi phase. [ABSTRACT FROM AUTHOR]